JP2014114350A - Curable coating composition, laminate polyester resin film and solar cell back sheet - Google Patents
Curable coating composition, laminate polyester resin film and solar cell back sheet Download PDFInfo
- Publication number
- JP2014114350A JP2014114350A JP2012268300A JP2012268300A JP2014114350A JP 2014114350 A JP2014114350 A JP 2014114350A JP 2012268300 A JP2012268300 A JP 2012268300A JP 2012268300 A JP2012268300 A JP 2012268300A JP 2014114350 A JP2014114350 A JP 2014114350A
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- JP
- Japan
- Prior art keywords
- coating composition
- resin
- inorganic filler
- film
- hydroxyl group
- 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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- 239000008199 coating composition Substances 0.000 title claims abstract description 43
- 239000004645 polyester resin Substances 0.000 title claims description 37
- 229920001225 polyester resin Polymers 0.000 title claims description 35
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 65
- 229920005989 resin Polymers 0.000 claims abstract description 48
- 239000011347 resin Substances 0.000 claims abstract description 48
- 239000011256 inorganic filler Substances 0.000 claims abstract description 39
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 39
- 150000001875 compounds Chemical class 0.000 claims abstract description 33
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 32
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 32
- -1 carbodiimide compound Chemical class 0.000 claims description 34
- 239000004925 Acrylic resin Substances 0.000 claims description 13
- 229920000178 Acrylic resin Polymers 0.000 claims description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 4
- 239000010456 wollastonite Substances 0.000 claims description 4
- 229910052882 wollastonite Inorganic materials 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 229920005668 polycarbonate resin Polymers 0.000 claims description 2
- 239000004431 polycarbonate resin Substances 0.000 claims description 2
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 2
- 239000004611 light stabiliser Substances 0.000 claims 1
- 229920006267 polyester film Polymers 0.000 claims 1
- 229920002799 BoPET Polymers 0.000 abstract description 23
- 239000000203 mixture Substances 0.000 abstract description 9
- 230000007062 hydrolysis Effects 0.000 abstract description 7
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 7
- 230000000903 blocking effect Effects 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 4
- 239000005001 laminate film Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 45
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 28
- 239000000049 pigment Substances 0.000 description 28
- 210000004027 cell Anatomy 0.000 description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 18
- 239000011248 coating agent Substances 0.000 description 18
- 238000000576 coating method Methods 0.000 description 18
- 239000000758 substrate Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 239000007787 solid Substances 0.000 description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 238000001723 curing Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 230000006866 deterioration Effects 0.000 description 9
- 229920001577 copolymer Polymers 0.000 description 8
- 238000010030 laminating Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000007789 sealing Methods 0.000 description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 7
- 125000003118 aryl group Chemical group 0.000 description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 description 7
- 239000005020 polyethylene terephthalate Substances 0.000 description 7
- 229920005672 polyolefin resin Polymers 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000004383 yellowing Methods 0.000 description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 6
- 239000005977 Ethylene Substances 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 230000009477 glass transition Effects 0.000 description 5
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 230000004224 protection Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 125000001931 aliphatic group Chemical group 0.000 description 4
- 239000002981 blocking agent Substances 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 4
- 238000002845 discoloration Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 229920002367 Polyisobutene Polymers 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 3
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000000378 calcium silicate Substances 0.000 description 3
- 229910052918 calcium silicate Inorganic materials 0.000 description 3
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010494 dissociation reaction Methods 0.000 description 3
- 230000005593 dissociations Effects 0.000 description 3
- 125000003438 dodecyl group Chemical group [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])* 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 150000002148 esters Chemical group 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-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
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000011112 polyethylene naphthalate Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 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
- 239000003981 vehicle Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- WULAHPYSGCVQHM-UHFFFAOYSA-N 2-(2-ethenoxyethoxy)ethanol Chemical compound OCCOCCOC=C WULAHPYSGCVQHM-UHFFFAOYSA-N 0.000 description 2
- VUIWJRYTWUGOOF-UHFFFAOYSA-N 2-ethenoxyethanol Chemical compound OCCOC=C VUIWJRYTWUGOOF-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- HMBNQNDUEFFFNZ-UHFFFAOYSA-N 4-ethenoxybutan-1-ol Chemical compound OCCCCOC=C HMBNQNDUEFFFNZ-UHFFFAOYSA-N 0.000 description 2
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 2
- 239000004606 Fillers/Extenders Substances 0.000 description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 229920003232 aliphatic polyester Polymers 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 125000005907 alkyl ester group Chemical group 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
- 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 2
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 125000001624 naphthyl group Chemical group 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 239000012860 organic pigment Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 2
- XUWHAWMETYGRKB-UHFFFAOYSA-N piperidin-2-one Chemical compound O=C1CCCCN1 XUWHAWMETYGRKB-UHFFFAOYSA-N 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000011342 resin composition Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
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- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 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 2
- 238000004381 surface treatment Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 235000014692 zinc oxide Nutrition 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
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- 239000002075 main ingredient Substances 0.000 description 1
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- SOOARYARZPXNAL-UHFFFAOYSA-N methyl-thiophenol Natural products CSC1=CC=CC=C1O SOOARYARZPXNAL-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- ZIYVHBGGAOATLY-UHFFFAOYSA-L methylmalonate(2-) Chemical compound [O-]C(=O)C(C)C([O-])=O ZIYVHBGGAOATLY-UHFFFAOYSA-L 0.000 description 1
- 125000002816 methylsulfanyl group Chemical group [H]C([H])([H])S[*] 0.000 description 1
- 239000000983 mordant dye Substances 0.000 description 1
- WHIVNJATOVLWBW-UHFFFAOYSA-N n-butan-2-ylidenehydroxylamine Chemical compound CCC(C)=NO WHIVNJATOVLWBW-UHFFFAOYSA-N 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
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- 150000002923 oximes Chemical class 0.000 description 1
- 235000012736 patent blue V Nutrition 0.000 description 1
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- DGBWPZSGHAXYGK-UHFFFAOYSA-N perinone Chemical compound C12=NC3=CC=CC=C3N2C(=O)C2=CC=C3C4=C2C1=CC=C4C(=O)N1C2=CC=CC=C2N=C13 DGBWPZSGHAXYGK-UHFFFAOYSA-N 0.000 description 1
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- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
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- 238000009832 plasma treatment Methods 0.000 description 1
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- 229920001627 poly(4-methyl styrene) Polymers 0.000 description 1
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- 229920003251 poly(α-methylstyrene) Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
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- 229920001748 polybutylene Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
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- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
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- 150000003346 selenoethers Chemical class 0.000 description 1
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- 150000004760 silicates Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- QXKXDIKCIPXUPL-UHFFFAOYSA-N sulfanylidenemercury Chemical compound [Hg]=S QXKXDIKCIPXUPL-UHFFFAOYSA-N 0.000 description 1
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- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
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- 238000004154 testing of material Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- JOUDBUYBGJYFFP-FOCLMDBBSA-N thioindigo Chemical compound S\1C2=CC=CC=C2C(=O)C/1=C1/C(=O)C2=CC=CC=C2S1 JOUDBUYBGJYFFP-FOCLMDBBSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 150000003852 triazoles Chemical class 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
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-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
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 235000013799 ultramarine blue Nutrition 0.000 description 1
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- 239000000984 vat dye Substances 0.000 description 1
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- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
Description
本発明は、硬化性コーティング組成物、積層ポリエステル樹脂フィルム及び太陽電池バックシートに関するものである。 The present invention relates to a curable coating composition, a laminated polyester resin film, and a solar battery back sheet.
本発明は、例えば鉄道車両、自動車、自動販売機等の表面に貼付して用いられるマーキング用フィルムの表面保護、光沢向上、変退色・劣化防止等を目的としたオーバーレイフィルムや、車両や住宅のプラスチック製ウインドウや外装看板の表面保護用フィルム、液晶ディスプレイ反射用シート、太陽電池用バックシート等として、主として保護や変退色防止の目的で用いられる高耐候性フィルム・シートに関するものである。
上記した高耐候性フィルム・シートは、共通して、物体を厳しい外部環境から遮断し保護することを目的としており、直射日光による紫外線暴露や大きな気温変化を受けたり、風雨に曝されるなどの環境変化があっても、長期間に亘り破れたりせずに、物体を確実に保護できることが必要となる。
例えば、太陽電池バックシートは、太陽電池本体を厳しい外部環境から遮断し保護することを目的としたシートである。太陽電池パネルは、屋外に設置されることから、直射日光による紫外線暴露や大きな気温変化および風雨に曝されるなどの環境変化があっても、長期間に亘り安定稼動することが必要である。当然、バックシート自体にも、耐UV性や耐候性が求められる。
この様な太陽電池バックシートに適用するポリエステル樹脂フィルムは、上記した厳しい品質を満足させるために、ポリエチレンテレフタレート(PET)やポリエチレンナフタレートの様なポリエステル樹脂中に、紫外線吸収剤、光安定剤等の添加剤を添加して混練し、必要な厚みとなる様に溶融押出成形するなどして製造されてきた。
しかしながら、上記した様な製造方法では、耐UV性や耐侯性にある程度優れたポリエステル樹脂フィルムは得られるものの、製造工程が多工程にわたり、簡便に得られないという欠点があった。
The present invention is, for example, an overlay film for the purpose of surface protection, improvement in gloss, prevention of discoloration / deterioration of a marking film used on a surface of a railway vehicle, automobile, vending machine, etc. The present invention relates to a highly weather-resistant film / sheet used mainly for the purpose of protection and prevention of discoloration, such as a surface protection film for plastic windows and exterior signs, a liquid crystal display reflection sheet, and a solar cell backsheet.
The above-mentioned high weather resistance films and sheets are commonly intended to shield and protect objects from harsh external environments. Even if there is an environmental change, it is necessary to be able to reliably protect an object without being broken for a long time.
For example, a solar cell back sheet is a sheet intended to shield and protect a solar cell body from a severe external environment. Since the solar cell panel is installed outdoors, it is necessary to operate stably over a long period of time even when there is an environmental change such as exposure to ultraviolet rays by direct sunlight, a large change in temperature, and exposure to wind and rain. Of course, the back sheet itself is also required to have UV resistance and weather resistance.
In order to satisfy the above-mentioned stringent quality, the polyester resin film applied to such a solar battery back sheet is not limited to a polyester resin such as polyethylene terephthalate (PET) or polyethylene naphthalate. These additives are added and kneaded, and melt extrusion is performed so as to obtain a required thickness.
However, the production method as described above has a drawback that although a polyester resin film having a certain degree of UV resistance and weather resistance can be obtained, the production process is multi-step and cannot be easily obtained.
また、PET(ポリエチレンテレフタラート)フィルムは機械的強度、耐熱性、光学特性、耐薬品性等の優れた特性を有しており、食品包材から工業用途まで幅広い分野で使用されている。しかしながら、その優れた特性の反面、紫外線による黄変劣化の欠点を有し、太陽電池バックシートなど屋外に長期間使用されるフィルムにおいては上記黄変劣化が使用限界の要因となっている。PETフィルムに紫外線カット性能を付与させるために、太陽電池バックシートの最外層に紫外線を吸収する汎用二酸化チタンを含有した硬化性コーティング組成物をPETフィルム上に施す方法が知られている。しかし、このような硬化性コーティング組成物は、PETフィルムとの密着性は塗工直後において優れるものの、高温高湿の環境下において密着性が著しく低下することが確認されている。 PET (polyethylene terephthalate) films have excellent properties such as mechanical strength, heat resistance, optical properties, and chemical resistance, and are used in a wide range of fields from food packaging materials to industrial applications. However, although it has excellent characteristics, it has a defect of yellowing deterioration due to ultraviolet rays, and the above-mentioned yellowing deterioration becomes a factor of use limit in a film used outdoors for a long time such as a solar battery backsheet. In order to impart UV-cutting performance to a PET film, a method is known in which a curable coating composition containing general-purpose titanium dioxide that absorbs UV light is applied to the PET film on the outermost layer of a solar cell backsheet. However, it has been confirmed that such a curable coating composition has an extremely low adhesion under a high temperature and high humidity environment, although the adhesion with a PET film is excellent immediately after coating.
一方、エポキシ樹脂を含有する硬化性コーティング組成物は、PETフィルムとの密着性は塗工直後や高温高湿の環境下において、密着性が維持されるといった開示も見受けられるが、エポキシ樹脂の紫外線耐性が弱いため、これを含有する硬化性コーティング組成物は黄変劣化を起こしやすい。これを防止するために、高価な紫外線吸収剤を添加する必要があり、製造コストアップが懸念される。
そこで、これらの課題を解決する硬化性コーティング組成物、積層ポリエステル樹脂フィルム及び太陽電池バックシートの開発が望まれている。
On the other hand, the curable coating composition containing an epoxy resin has been disclosed that the adhesion to the PET film is maintained immediately after coating or in an environment of high temperature and high humidity. Since resistance is weak, the curable coating composition containing this tends to cause yellowing deterioration. In order to prevent this, it is necessary to add an expensive ultraviolet absorber, and there is a concern about an increase in manufacturing cost.
Then, development of the curable coating composition, laminated polyester resin film, and solar cell back sheet which solve these subjects is desired.
従って、本発明の目的は、市販されている多様なPETフィルムにコーティングを施すことで、例えば、PETフィルムとの密着性、耐光性、耐ブロッキング性、耐侯性、貯蔵安定性、更には耐加水分解性を付与できる硬化性コーティング組成物を提供することである。 Therefore, an object of the present invention is to apply various PET films on the market, for example, adhesion to PET film, light resistance, blocking resistance, weather resistance, storage stability, and further resistance to water. It is to provide a curable coating composition capable of imparting degradability.
本発明者は、前記の課題を解決するため、鋭意検討の結果、水酸基を含有する樹脂とポリイソシアネート化合物とを含有する組成物に、アスペクト比が高い針状充填物を加えることにより、前記課題を解決することを見出した。 In order to solve the above-mentioned problems, the present inventor, as a result of intensive studies, added a needle-shaped filler having a high aspect ratio to the composition containing a resin containing a hydroxyl group and a polyisocyanate compound, thereby obtaining the above-mentioned problem. Found to solve.
すなわち本発明は、水酸基を含有する樹脂と、有機ポリイソシアネート化合物と、無機充填物を含有する硬化性コーティング組成物であって、前記無機充填物として、アスペクト比が5〜50である針状無機充填物を含有することを特徴とする硬化性コーティング組成物、該組成物を積層した積層フィルム、太陽電池バックシートを提供する。 That is, the present invention is a curable coating composition containing a hydroxyl group-containing resin, an organic polyisocyanate compound, and an inorganic filler, wherein the inorganic filler has an acicular inorganic aspect ratio of 5 to 50 Provided are a curable coating composition containing a filler, a laminated film obtained by laminating the composition, and a solar battery backsheet.
本発明の硬化性表面コーティング組成物によれば、市販されている多様のPETフィルムにコーティングを施すことで、紫外線吸収剤を用いなくても、前記PETフィルムに耐UV性や密着性、特に、高温高湿試験後の前記PETフィルムとの間に優れた密着性を付与できる。このため、従来手法のエポキシ樹脂に起因する黄変劣化を未然に防ぐことができる。また、これを用いた太陽電池バックシートを提供できる。 According to the curable surface coating composition of the present invention, by applying a coating to various commercially available PET films, UV resistance and adhesion to the PET film without using an ultraviolet absorber, in particular, Excellent adhesion can be imparted to the PET film after the high temperature and high humidity test. For this reason, the yellowing deterioration resulting from the epoxy resin of the conventional method can be prevented beforehand. Moreover, the solar cell backsheet using this can be provided.
本発明に用いる水酸基を含有する樹脂(A)としては、イソシアネート基と反応性を有する水酸基を含有する水酸基を含有する樹脂であれば、特に限定されないが、例えば、樹脂の水酸基価が1〜200mgKOH/gであることが好ましい。これらの樹脂としては、たとえば、それぞれ水酸基を有するアクリル樹脂、ポリエステル樹脂、ウレタン樹脂、ポリオレフィン樹脂又はフッ素樹脂等が挙げられ、これらは単独で、或いは、2種以上を併用してもよい。 The hydroxyl group-containing resin (A) used in the present invention is not particularly limited as long as it is a resin containing a hydroxyl group having a reactivity with an isocyanate group. For example, the hydroxyl value of the resin is 1 to 200 mgKOH. / G is preferable. Examples of these resins include an acrylic resin having a hydroxyl group, a polyester resin, a urethane resin, a polyolefin resin, or a fluorine resin, and these may be used alone or in combination of two or more.
前記水酸基を含有する樹脂(A)は、水酸基価が1〜200mgKOH/gであることが好ましいが、特に、水酸基価4〜100mgKOH/gの範囲にあることが、基材との密着性、耐久性および耐加水分解性の観点から好ましい。水酸基価が1より小さい場合は、塗膜の硬化がほとんど進まず、基材、例えばPETフィルムとの密着性、耐久性が劣ったり、水酸基価が200より大きい場合は、硬化収縮が大きすぎる為に、基材、例えばPETフィルムとの密着性が悪化したりする傾向にある。 The hydroxyl group-containing resin (A) preferably has a hydroxyl value of 1 to 200 mgKOH / g, and particularly preferably has a hydroxyl value in the range of 4 to 100 mgKOH / g. From the viewpoints of water resistance and hydrolysis resistance. When the hydroxyl value is less than 1, curing of the coating film hardly progresses, and adhesion and durability with a base material such as a PET film are inferior. When the hydroxyl value is more than 200, curing shrinkage is too large. In addition, the adhesion to a substrate such as a PET film tends to deteriorate.
本発明で用いられる水酸基を含有するアクリル樹脂とは、アクリル酸エステルまたはメタクリル酸エステルを必須成分として重合して得られる、水酸基を含有する線状樹脂をいう。以下、アクリルとメタクリルを合わせて(メタ)アクリルと称する。 The acrylic resin containing a hydroxyl group used in the present invention refers to a linear resin containing a hydroxyl group obtained by polymerizing an acrylic ester or a methacrylic ester as an essential component. Hereinafter, acrylic and methacryl are collectively referred to as (meth) acryl.
この様なアクリル樹脂は、例えば、(メタ)アクリル酸エステルを必須成分として、必要に応じて(メタ)アクリル酸、イタコン酸、無水マレイン酸等のカルボキシル酸基含有モノマーを共重合することで容易に製造することが出来る。(メタ)アクリル酸エステルとしては、例えば、メチル(メタ)アクリレート、エチル(メタ)アクリレート、プロピル(メタ)アクリレート、イソプロピル(メタ)アクリレート、ブチル(メタ)アクリレート、イソブチル(メタ)アクリレート、tert−ブチル(メタ)アクリレート、ラウリル(メタ)アクリレート、ステアリル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、シクロヘキシル(メタ)アクリレート、メチルシクロヘキシル(メタ)アクリレート、シクロドデシル(メタ)アクリレート、イソボルニル(メタ)アクリレートなどが挙げられる。 Such an acrylic resin can be easily obtained, for example, by copolymerizing a carboxylic acid group-containing monomer such as (meth) acrylic acid, itaconic acid, maleic anhydride, etc. as necessary with (meth) acrylic acid ester as an essential component. Can be manufactured. Examples of (meth) acrylic acid esters include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, and tert-butyl. (Meth) acrylate, lauryl (meth) acrylate, stearyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, cyclohexyl (meth) acrylate, methylcyclohexyl (meth) acrylate, cyclododecyl (meth) acrylate, isobornyl (meth) acrylate Etc.
(メタ)アクリル酸エステルを必須成分として、共重合を行うに当たり、例えば、ヒドロキシエチル(メタ)アクリレート、ヒドロキシプロピル(メタ)アクリレート、ヒドロキシブチル(メタ)アクリレートなどの水酸基含有(メタ)アクリル酸エステルを併用することで、アクリル樹脂骨格の側鎖に水酸基が導入された、水酸基含有(メタ)アクリル樹脂を得ることができる。 In carrying out copolymerization using (meth) acrylic acid ester as an essential component, for example, hydroxyl-containing (meth) acrylic acid ester such as hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, hydroxybutyl (meth) acrylate, etc. By using together, the hydroxyl-containing (meth) acrylic resin by which the hydroxyl group was introduce | transduced into the side chain of the acrylic resin frame | skeleton can be obtained.
この様な水酸基を含有するアクリル樹脂は、線状であることによる、低粘度、硬化皮膜の優れた可撓性等の特徴を大きく損なわない範囲において、前記した単量体に、エチレングリコールジ(メタ)アクリレート、トリメチロールプロパントリ(メタ)アクリレート、ヘキサ(メタ)アクリレートの様な、2〜6個の(メタ)アクリロイル基を含有する重合性単量体を少量併用して重合したアクリル樹脂であっても良い。 An acrylic resin containing such a hydroxyl group has an ethylene glycol di () content in the above-mentioned monomer within a range that does not greatly impair characteristics such as low viscosity due to being linear and excellent flexibility of the cured film. It is an acrylic resin that is polymerized with a small amount of 2-6 (meth) acryloyl group-containing polymerizable monomers such as (meth) acrylate, trimethylolpropane tri (meth) acrylate, and hexa (meth) acrylate. There may be.
この様な水酸基を含有するアクリル樹脂としては、例えば、DIC(株)製「アクリディック」シリーズ、大成ファインケミカル(株)製「アクリット」シリーズがある。例えば、アクリル樹脂の市販品としては、DIC(株)製、商品名:アクリディックA−808−T、同57−451を挙げることが出来る。 Examples of such an acrylic resin containing a hydroxyl group include “Acridic” series manufactured by DIC Corporation and “Aclit” series manufactured by Taisei Fine Chemical Co., Ltd. For example, as a commercial item of an acrylic resin, DIC Corporation make, brand name: ACRYDIC A-808-T, 57-451 can be mentioned.
本発明に用いる水酸基を含有するポリエステル樹脂とは、グリコールと、二塩基酸またはその誘導体とを必須成分として反応させて得られる、過剰の水酸基を含有する線状樹脂をいう。勿論、上記二塩基酸に代えて、二塩基酸無水物、二塩基酸低級アルキルエステル等のエステル形成性誘導体を用いて、重縮合反応のみならず、付加反応やエステル交換反応にて、ポリエステル樹脂を得ることも出来る。 The polyester resin containing a hydroxyl group used in the present invention refers to a linear resin containing an excess hydroxyl group obtained by reacting glycol with dibasic acid or a derivative thereof as essential components. Of course, in place of the dibasic acid, an ester-forming derivative such as a dibasic acid anhydride or a dibasic acid lower alkyl ester is used, and not only in a polycondensation reaction, but also in an addition reaction or an ester exchange reaction, Can also be obtained.
ポリエステル樹脂としては、例えばエチレングリコール、プロピレングリコール、ブタンジオール、ペンタンジオール、ヘキサンジオール、ヘプタンジオール、デカンジオール、シクロヘキサンジメタノール等の脂肪族グリコールと、例えばコハク酸、アジピン酸、セバシン酸、フマル酸スベリン酸、アゼライン酸、1,10−デカメチレンジカルボン酸、シクロヘキサンジカルボン酸等の脂肪族ニ塩基酸とを必須原料成分として反応させた脂肪族ポリエステル樹脂や、エチレングリコール、プロピレングリコール、ブタンジオール等の脂肪族グリコールと、例えば、テレフタル酸、イソフタル酸、ナフタレンジカルボン酸等の芳香族二塩基酸とを必須原料成分として反応させた芳香族ポリエステル樹脂が挙げられる。 Examples of the polyester resin include aliphatic glycols such as ethylene glycol, propylene glycol, butanediol, pentanediol, hexanediol, heptanediol, decanediol, and cyclohexanedimethanol, and succinic acid, adipic acid, sebacic acid, and suberin fumarate. Aliphatic polyester resins obtained by reacting acid, azelaic acid, aliphatic dibasic acid such as 1,10-decamethylenedicarboxylic acid and cyclohexanedicarboxylic acid as essential raw material components, and fats such as ethylene glycol, propylene glycol and butanediol An aromatic polyester resin obtained by reacting an aromatic glycol with an aromatic dibasic acid such as terephthalic acid, isophthalic acid, naphthalenedicarboxylic acid or the like as an essential raw material component can be given.
この様な水酸基を含有するポリエステル樹脂は、線状であることによる、低粘度、硬化皮膜の優れた可撓性等の特徴を大きく損なわない範囲において、前記したグリコールや二塩基酸に、トリメリット酸、ピロメリット酸、トロメチロールプロパン、ペンタエリスルトール等の、水酸基やカルボシキル基等の活性水素基を分子内に3〜4個含有する化合物を少量併用して得たポリエステル樹脂であっても良い。 Such a hydroxyl group-containing polyester resin has a trimerit to glycols and dibasic acids as long as the characteristics such as low viscosity and excellent flexibility of the cured film are not greatly impaired. Even a polyester resin obtained by using a small amount of a compound containing 3 to 4 active hydrogen groups such as hydroxyl group or carboxy group such as acid, pyromellitic acid, tromethylolpropane and pentaerythritol in the molecule good.
前記ポリエステル樹脂は、その主鎖中にベンゼン環やナフタレン環がより多く含有されることでTgがより高くなる傾向があり、例えば、コーティングすべき対象基材がPETやPBT(ポリブチレンテレフタレート)やPEN(ポリエチレンナフタレート)との親和性が高まるため、本発明では脂肪族ポリエステル樹脂よりも芳香族ポリエステル樹脂を用いることが好ましい。しかしながら、主鎖中にベンゼン環やナフタレン環がより多く含有されることで、結晶性や融点等も高くなる傾向があり、流動性や塗布性が低下しやすい。 The polyester resin tends to have a higher Tg by containing more benzene rings and naphthalene rings in the main chain. For example, the target substrate to be coated is PET, PBT (polybutylene terephthalate), Since affinity with PEN (polyethylene naphthalate) increases, it is preferable to use an aromatic polyester resin rather than an aliphatic polyester resin in the present invention. However, since more benzene rings and naphthalene rings are contained in the main chain, crystallinity, melting point, etc. tend to increase, and fluidity and applicability tend to be lowered.
そのため、前記ポリエステル樹脂は、示差走査熱量分析法(DSC法)でのガラス転移温度(Tg)20〜110℃のポリエステル樹脂であることが好ましい。本発明では、全アルコール中炭素原子数2〜4の脂肪族グリコール25モル%以上を用い、かつ全多塩基酸中芳香族二塩基酸30モル%以上を用いて得た、Tgが40〜100℃の芳香族ポリエステル樹脂を用いることがより好ましい。 Therefore, the polyester resin is preferably a polyester resin having a glass transition temperature (Tg) of 20 to 110 ° C. according to differential scanning calorimetry (DSC method). In the present invention, Tg of 40 to 100 obtained by using 25 mol% or more of aliphatic glycol having 2 to 4 carbon atoms in all alcohols and 30 mol% or more of aromatic dibasic acid in all polybasic acids. It is more preferable to use an aromatic polyester resin at ° C.
水酸基を含有するポリエステル樹脂としては、例えば、東洋紡績(株)製「バイロン」シリーズ、ユニチカ(株)製「エリーテル」シリーズ、更に詳しくは、例えばユニチカ(株)製、商品名:エリーテルUE−3210、同XA−0611が挙げられる。 Examples of the polyester resin containing a hydroxyl group include “Byron” series manufactured by Toyobo Co., Ltd., “Eritel” series manufactured by Unitika Ltd., and more specifically, for example, manufactured by Unitika Ltd., trade name: Elitel UE-3210. XA-0611.
本発明に用いる水酸基を含有するポリウレタン樹脂とは、たとえば、ポリイソシアネート化合物と1分子中に少なくとも2個の水酸基を含有する化合物とを、水酸基がイソシアネート基に対して過剰となるような比率で反応させて得られる。その際に使用されるポリイソシアネート化合物としては、ヘキサメチレンジイソシアネート、トルエンジイソシアネート、m−キシリレンジイソシアネート、イソホロンジイソシアネート等が挙げられる。また、1分子中に少なくとも2個の水酸基を含有する化合物としては、前記多価アルコール類、ポリエステルジオール、ポリエチレングリコール、ポリプロピレングリコール、ポリカーボネートジオール等が挙げられる。 With the polyurethane resin containing a hydroxyl group used in the present invention, for example, a polyisocyanate compound and a compound containing at least two hydroxyl groups in one molecule are reacted at a ratio such that the hydroxyl group is excessive with respect to the isocyanate group. Can be obtained. Examples of the polyisocyanate compound used at that time include hexamethylene diisocyanate, toluene diisocyanate, m-xylylene diisocyanate, and isophorone diisocyanate. Examples of the compound containing at least two hydroxyl groups in one molecule include the polyhydric alcohols, polyester diol, polyethylene glycol, polypropylene glycol, and polycarbonate diol.
本発明に用いられる水酸基を含有するポリオレフィン樹脂とは、ポリオレフィン樹脂を後述する水酸基含有(メタ)アクリル酸エステル、あるいは、水酸基含有ビニルエーテルでグラフト変性あるいは共重合化し、合成される。
ポリオレフィン樹脂としては、炭素数2〜8のオレフィンの単独重合体や共重合体、炭素数2〜8のオレフィンと他のモノマーとの共重合体を挙げることができる。具体的には、例えば、高密度ポリエチレン(HDPE)、低密度ポリエチレン(LDPE)、線状低密度ポリエチレン樹脂などのポリエチレン、ポリプロピレン、ポリイソブチレン、ポリ(1−ブテン)、ポリ4−メチルペンテン、ポリビニルシクロヘキサン、ポリスチレン、ポリ(p−メチルスチレン)、ポリ(α−メチルスチレン)、エチレン・プロピレンブロック共重合体、エチレン・プロピレンランダム共重合体、エチレン・ブテン−1共重合体、エチレン・4−メチル−1−ペンテン共重合体、エチレン・へキセン共重合体などのα―オレフィン共重合体、エチレン・酢酸ビニル共重合体、エチレン・アクリル酸共重合体、エチレン・メチルメタクリレート共重合体、エチレン・酢酸ビニル・メチルメタクリレート共重合体、アイオノマー樹脂などを挙げることができる。更に、これらポリオレフィンを塩素化した塩素化ポリオレフィンも使用することができる。
The polyolefin resin containing a hydroxyl group used in the present invention is synthesized by graft-modifying or copolymerizing a polyolefin resin with a hydroxyl group-containing (meth) acrylic acid ester or a hydroxyl group-containing vinyl ether described later.
Examples of the polyolefin resin include homopolymers and copolymers of olefins having 2 to 8 carbon atoms, and copolymers of olefins having 2 to 8 carbon atoms and other monomers. Specifically, for example, high density polyethylene (HDPE), low density polyethylene (LDPE), polyethylene such as linear low density polyethylene resin, polypropylene, polyisobutylene, poly (1-butene), poly-4-methylpentene, polyvinyl Cyclohexane, polystyrene, poly (p-methylstyrene), poly (α-methylstyrene), ethylene / propylene block copolymer, ethylene / propylene random copolymer, ethylene / butene-1 copolymer, ethylene / 4-methyl -1-pentene copolymer, α-olefin copolymer such as ethylene / hexene copolymer, ethylene / vinyl acetate copolymer, ethylene / acrylic acid copolymer, ethylene / methyl methacrylate copolymer, ethylene / Vinyl acetate methyl methacrylate copolymer, Aio Examples thereof include nomer resins. Furthermore, chlorinated polyolefins obtained by chlorinating these polyolefins can also be used.
前記水酸基含有(メタ)アクリル酸エステルとしては、(メタ)アクリル酸ヒドロキエチル;(メタ)アクリル酸ヒドロキシプロピル、(メタ)アクリル酸グリセロール;ラクトン変性(メタ)アクリル酸ヒドロキシエチル、(メタ)アクリル酸ポリエチレングリコール、(メタ)アクリル酸ポリプロピレングリコール等が挙げられ、前記水酸基含有ビニルエーテルとしては、2−ヒドロキシエチルビニルエーテル、ジエチレングリコールモノビニルエーテル、4−ヒドロキシブチルビニルエーテル等が挙げられる。 Examples of the hydroxyl group-containing (meth) acrylic acid ester include hydroxyethyl (meth) acrylate; hydroxypropyl (meth) acrylate, glycerol (meth) acrylate; lactone modified hydroxyethyl (meth) acrylate, (meth) acrylic acid. Examples include polyethylene glycol and polypropylene glycol (meth) acrylic acid, and examples of the hydroxyl group-containing vinyl ether include 2-hydroxyethyl vinyl ether, diethylene glycol monovinyl ether, and 4-hydroxybutyl vinyl ether.
これらの水酸基を含有するポリオレフィン樹脂としては、例えば、三井化学(株)製、「ユニストール」などが市販されている。 As the polyolefin resin containing these hydroxyl groups, for example, “Unistol” manufactured by Mitsui Chemicals, Inc. is commercially available.
本発明で用いられる水酸基を含有するフッ素樹脂とは、フッ素ビニル単量体を必須成分として重合して得られる、水酸基を含有する線状樹脂をいう。 The fluororesin containing a hydroxyl group used in the present invention refers to a linear resin containing a hydroxyl group obtained by polymerizing a fluorovinyl monomer as an essential component.
上記したフッ素ビニル単量体としては、例えば、フッ化ビニル、フッ化ビニリデン、テトラフルオロエチレン、ヘキサフルオロプロピレン、1,1,3,3,3−ペンタフルオロプロピレン、2,2,3,3−テトラフルオロプロピレン、1,1,2−トリフルオロプロピレンまたは3,3,3−トリフルオロプロピレンの如き、純粋なる意味でのフルオロオレフィンをはじめ、さらには、クロロトリフルオロエチレン、ブロモトリフルオロエチレン、1−クロロ−1,2−ジフルオロエチレンまたは1,1−ジクロロ−2,2−ジフルオロエチレンの如き、フッ素原子以外のハロゲン原子をも有する形の化合物までを包含した、いわゆる広義のフルオロオレフィン類などが挙げられる。 Examples of the fluorine vinyl monomer include vinyl fluoride, vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene, 1,1,3,3,3-pentafluoropropylene, 2,2,3,3- Including pure fluoroolefins such as tetrafluoropropylene, 1,1,2-trifluoropropylene or 3,3,3-trifluoropropylene, chlorotrifluoroethylene, bromotrifluoroethylene, 1 -So-called fluoroolefins in a broad sense including compounds having a halogen atom other than a fluorine atom such as chloro-1,2-difluoroethylene or 1,1-dichloro-2,2-difluoroethylene Can be mentioned.
更に、フッ素樹脂の必須成分として、共重合を行うに当たり、例えば、ヒドロキシエチル(メタ)アクリレート、ヒドロキシプロピル(メタ)アクリレート、ヒドロキシブチル(メタ)アクリレートなどの水酸基含有(メタ)アクリル酸エステル、あるいは、2−ヒドロキシエチルビニルエーテル、ジエチレングリコールモノビニルエーテル、4−ヒドロキシブチルビニルエーテルなどの水酸基含有ビニルエーテルを併用することで、フッ素樹脂骨格の側鎖に水酸基が導入された、水酸基を含有するフッ素樹脂を得ることができる。水酸基を含有するフッ素樹脂としては、例えば、DIC(株)製「フルオネート」シリーズなどが挙げられる。 Furthermore, as an essential component of the fluororesin, for copolymerization, for example, hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, hydroxyl-containing (meth) acrylate such as hydroxybutyl (meth) acrylate, or By using together a hydroxyl group-containing vinyl ether such as 2-hydroxyethyl vinyl ether, diethylene glycol monovinyl ether, 4-hydroxybutyl vinyl ether, etc., a hydroxyl group-containing fluororesin having a hydroxyl group introduced into the side chain of the fluororesin skeleton can be obtained. . Examples of the fluororesin containing a hydroxyl group include “Fluonate” series manufactured by DIC Corporation.
本発明で用いる水酸基を含有する樹脂(A)は、数平均分子量5,000〜50,000を満たすこと、好ましくは数平均分子量10,000〜30,000であることが、PETフィルムとの密着性、耐加水分解性に優れる点でより好ましい。上記した分子量の水酸基を含有する樹脂は、有機溶剤に溶解する上、同溶液の流動性を大きくは損なうことなく、際立ったPETフィルムとの密着性や耐加水分解性を発現する。 The resin (A) containing a hydroxyl group used in the present invention satisfies the number average molecular weight of 5,000 to 50,000, preferably the number average molecular weight of 10,000 to 30,000. It is more preferable in terms of excellent properties and hydrolysis resistance. The above-described resin containing a hydroxyl group having a molecular weight dissolves in an organic solvent, and exhibits outstanding adhesion to a PET film and hydrolysis resistance without greatly impairing the fluidity of the solution.
本発明で用いる水酸基を含有する樹脂(A)は、プラスチックフィルムの様な可とう性の基材上で密着性に優れる塗膜を形成させる為に、ガラス転移温度20〜110℃を満たすこと、特に、ガラス転移温度40〜100℃であることがより好ましい。上記したガラス転移温度の水酸基を含有する樹脂は、PETフィルムとの接着性、耐ブロッキング性、耐加水分解性をバランスよく満たすことができる。 The resin (A) containing a hydroxyl group used in the present invention satisfies a glass transition temperature of 20 to 110 ° C. in order to form a coating film having excellent adhesion on a flexible substrate such as a plastic film. In particular, the glass transition temperature is more preferably 40 to 100 ° C. The above-mentioned resin containing a hydroxyl group having a glass transition temperature can satisfy a good balance of adhesion to a PET film, blocking resistance, and hydrolysis resistance.
本発明で用いられるポリイソシアネート化合物(B)としては、イソシアネート基を分子内に少なくとも2つ有する有機化合物が挙げられる。有機ポリイソシアネート化合物としては、例えば、トリレンジイソシアネート、キシリレンジイソシアネート、ジフェニルメタンジイソシアネート、1,6−ヘキサメチレンジイソシアネート、イソホロンジイソシアネート、4,4’−メチレンビス(シクロヘキシルイソシアネート)、リジンジイソシアネート、トリメチルヘキサメチレンジイソシアネート、1,3−(イソシアナートメチル)シクロヘキサン、1,5−ナフタレンジイソシアネート、トリフェニルメタントリイソシアネートなどのポリイソシアネート;これらのポリイソシアネートのアダクト体、ビュレット体、イソシアヌレート体などのポリイソシアネートの誘導体(変性物)などが挙げられる。 Examples of the polyisocyanate compound (B) used in the present invention include organic compounds having at least two isocyanate groups in the molecule. Examples of the organic polyisocyanate compound include tolylene diisocyanate, xylylene diisocyanate, diphenylmethane diisocyanate, 1,6-hexamethylene diisocyanate, isophorone diisocyanate, 4,4′-methylenebis (cyclohexyl isocyanate), lysine diisocyanate, trimethylhexamethylene diisocyanate, Polyisocyanates such as 1,3- (isocyanatomethyl) cyclohexane, 1,5-naphthalene diisocyanate, triphenylmethane triisocyanate; derivatives of polyisocyanates such as adducts, burettes and isocyanurates of these polyisocyanates (modified) Etc.).
本発明に用いるポリイソシアネート化合物(B)は、使用される用途によって適宜選択すれば良いが、トリレンジイソシアネートの様な芳香族系は黄変する場合があり、より優れた耐候性を要する場合には、脂肪族系または脂環式等の無黄変型ポリイソシアネートを用いることが好ましい。ポリエステル樹脂フィルムの様な透明な基材上で硬化塗膜が着色して透明性が低下するのは視認性悪化の点でも好ましくない。よって本発明で好適なのは、脂肪族または脂環式等の無黄変型ポリイソシアネートである、例えば、ヘキサメチレンジイソシアネート(HDI)、イソホロンジイソシアネート(IPDI)等の無黄変型ポリイソシアネートを用いることが好ましい。 The polyisocyanate compound (B) used in the present invention may be appropriately selected depending on the application to be used, but an aromatic system such as tolylene diisocyanate may turn yellow and requires better weather resistance. Is preferably an aliphatic or alicyclic non-yellowing polyisocyanate. It is not preferable that the cured coating film is colored on a transparent substrate such as a polyester resin film and the transparency is lowered in view of deterioration of visibility. Therefore, it is preferable to use non-yellowing polyisocyanates such as aliphatic or alicyclic non-yellowing polyisocyanates such as hexamethylene diisocyanate (HDI) and isophorone diisocyanate (IPDI).
前記硬化剤は、ポリイソシアネート化合物(B)のみでもある程度の性能が発現するが、ポリイソシアネート化合物とポリカーボネート樹脂及び/又はカルボジイミド化合物とを積極的に併用することより、硬化塗膜により高度な耐加水分解性を付与することが出来る。 The curing agent exhibits a certain level of performance only with the polyisocyanate compound (B). However, since the polyisocyanate compound is used in combination with a polycarbonate resin and / or a carbodiimide compound, the cured coating film has a higher water resistance. Degradability can be imparted.
前記水酸基を含有する樹脂(A)とポリイソシアネート化合物(B)との配合割合は、水酸基を含有する樹脂(A)の固形分水酸基当量(a)とポリイソシアネート化合物(B)の固形分イソシアネート当量(b)の当量比〔(a)/(b)〕が0.5〜5、好ましくは、0.8〜2.0であることが好ましい。 The mixing ratio of the hydroxyl group-containing resin (A) and the polyisocyanate compound (B) is such that the hydroxyl group-containing resin (A) has a solid content hydroxyl equivalent (a) and the polyisocyanate compound (B) has a solid content isocyanate equivalent. The equivalent ratio [(a) / (b)] of (b) is 0.5 to 5, preferably 0.8 to 2.0.
さらに、本発明に用いるポリイソシアネート化合物はブロック化ポリイソシアネートであっても良い。 Furthermore, the polyisocyanate compound used in the present invention may be a blocked polyisocyanate.
ブロック化剤としては、例えばフェノール、チオフェノール、メチルチオフェノール、キシレノール、クレゾール、レゾルシノール、ニトロフェノール、クロロフェノール等のフェノール類、アセトンオキシム、メチルエチルケトンオキシム、シクロヘキサノンオキシム等のオキシム類、メタノール、エタノール、n−プロピルアルコール、イソプロピルアルコール、n−ブチルアルコール、イソブチルアルコール、t−ブチルアルコール、t−ペンタノール、エチレングリコールモノエチルエーテル、エチレングリコールモノブチルエーテル、ジエチレングリコールモノエチルエーテル、プロピレングリコールモノメチルエーテル、ベンジルアルコールなどのアルコール類、3、5−ジメチルピラゾール、1、2−ピラゾール等のピラゾール類、1、2、4−トリアゾール等のトリアゾール類、エチレンクロルヒドリン、1、3−ジクロロ−2−プロパノール等のハロゲン置換アルコール類、ε−カプロラクタム、δ−バレロラクタム、γ−ブチロラクタム、β−プロピルラクタム等のラクタム類、アセト酢酸メチル、アセト酢酸エチル、アセチルアセトン、マロン酸メチル、マロン酸エチル等の活性メチレン化合物類が挙げられる。その他にもアミン類、イミド類、メルカプタン類、イミン類、尿素類、ジアリール類等も挙げられる。 Examples of the blocking agent include phenols such as phenol, thiophenol, methylthiophenol, xylenol, cresol, resorcinol, nitrophenol, chlorophenol, oximes such as acetone oxime, methyl ethyl ketone oxime, cyclohexanone oxime, methanol, ethanol, n- Alcohols such as propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutyl alcohol, t-butyl alcohol, t-pentanol, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monoethyl ether, propylene glycol monomethyl ether, benzyl alcohol Pyrazo such as 3,5-dimethylpyrazole, 1,2-pyrazole , Triazoles such as 1,2,4-triazole, halogen substituted alcohols such as ethylene chlorohydrin, 1,3-dichloro-2-propanol, ε-caprolactam, δ-valerolactam, γ-butyrolactam, β- Examples include lactams such as propyl lactam, and active methylene compounds such as methyl acetoacetate, ethyl acetoacetate, acetylacetone, methyl malonate, and ethyl malonate. Other examples include amines, imides, mercaptans, imines, ureas, and diaryls.
これらのブロック剤の中でも、ブロック剤の解離温度が80℃〜140℃のものが好ましい。解離温度が80℃未満であると、高温な貯蔵所において、ブロック剤がポリイソシアネートから解離する危険性があり、1液タイプとして設計された硬化性コーティング組成物の貯蔵安定性が損なわれる危険性がある。また、解離温度が150℃を超えると、太陽電池モジュールを構成する際の真空熱圧着の工程で、硬化反応が充分に進行せず、PETフィルム基材、封止層との密着性が低下してしまう。 Among these blocking agents, those having a dissociation temperature of 80 to 140 ° C. are preferable. When the dissociation temperature is less than 80 ° C., there is a risk that the blocking agent will dissociate from the polyisocyanate in a high-temperature storage, and the storage stability of the curable coating composition designed as a one-component type may be impaired. There is. In addition, when the dissociation temperature exceeds 150 ° C., the curing reaction does not sufficiently proceed in the vacuum thermocompression bonding step when configuring the solar cell module, and the adhesion with the PET film substrate and the sealing layer is reduced. End up.
この様なブロック剤を含有するポリイソシアネートとしては、例えば、旭化成ケミカルズ(株)製「デュラネート」シリーズ、住友バイエルウレタン(株)製「デスモジュール」シリーズがある。更に詳しくは、例えば住友バイエルウレタン(株)製、商品名:デュラネートTPA−B80Eが挙げられる。 Examples of the polyisocyanate containing such a blocking agent include “Duranate” series manufactured by Asahi Kasei Chemicals Corporation, and “Death Module” series manufactured by Sumitomo Bayer Urethane Co., Ltd. More specifically, for example, trade name: Duranate TPA-B80E manufactured by Sumitomo Bayer Urethane Co., Ltd. may be mentioned.
本発明に用いる無機充填物は、アスペクト比が5〜100である針状無機充填物が必須成分として含有していれば、特に限定されないが、例えば、酸化チタン、チタン酸カリウム、ウォラストナイト、酸化ジルコニウム、酸化亜鉛等の金属酸化物、ケイ酸カルシウム、炭酸カルシウム、ベーマイト、ホウ酸アルミニウム、ケイ酸カルシウム、塩基性硫酸マグネシウム、硫酸カルシウム、炭酸カルシウム、ホウ酸アルミニウム、硝酸マグネシウム等の金属化合物等が挙げられ、これらの中でも、チタン酸カリウムウィスカ、ウォラストナイトウィスカ、針状酸化チタンが好ましい。 The inorganic filler used in the present invention is not particularly limited as long as the acicular inorganic filler having an aspect ratio of 5 to 100 is contained as an essential component. For example, titanium oxide, potassium titanate, wollastonite, Metal oxides such as zirconium oxide and zinc oxide, metal compounds such as calcium silicate, calcium carbonate, boehmite, aluminum borate, calcium silicate, basic magnesium sulfate, calcium sulfate, calcium carbonate, aluminum borate, magnesium nitrate, etc. Among these, potassium titanate whisker, wollastonite whisker, and acicular titanium oxide are preferable.
なお、本願において、アスペクト比とは、針状無機充填物の長軸の短軸に対する長さの比であることを意味する。 In the present application, the aspect ratio means the ratio of the length of the major axis of the acicular inorganic filler to the minor axis.
前記針状無機充填物の配合比率としては、例えば、水酸基を含有する樹脂(A)と、有機ポリイソシアネート化合物(B)の合計100重量部(固形分)に対して、 〜 重量部配合することが好ましい。 As a blending ratio of the needle-like inorganic filler, for example, ~ 100 parts by weight are blended with respect to 100 parts by weight (solid content) of the resin (A) containing a hydroxyl group and the organic polyisocyanate compound (B). Is preferred.
また、本発明の硬化性コーティング組成物には、前記針状無機充填物以外の無機充填物を適宜配合してもよい。これらの充填物としては、例えば、前記の針状無機充填剤のアスペクト比が低い物質、或いは、塗料原料便覧1970年度版(日本塗料工業会編)に記載されている体質顔料、白顔料、黒顔料、灰色顔料、赤色顔料、茶色顔料、緑色顔料、青顔料、金属粉顔料、発光顔料、真珠色顔料等の有機顔料や無機顔料、さらにはプラスチック顔料などが挙げられる。これら着色剤の具体例としては種々のものが掲げられ、有機顔料としては、例えば、ベンチジンエロー、ハンザエロー、レーキッド4R等の、各種の不溶性アゾ顔料;レーキッドC、カーミン6B、ボルドー10等の如き溶性アゾ顔料; Moreover, you may mix | blend inorganic fillers other than the said acicular inorganic filler suitably with the curable coating composition of this invention. These fillers include, for example, substances having a low aspect ratio of the above-mentioned acicular inorganic fillers, or extender pigments, white pigments, black pigments described in the Paint Material Handbook 1970 edition (edited by the Japan Paint Industry Association) Examples thereof include organic pigments and inorganic pigments such as pigments, gray pigments, red pigments, brown pigments, green pigments, blue pigments, metal powder pigments, luminescent pigments and pearl pigments, and plastic pigments. Specific examples of these colorants are listed, and examples of organic pigments include various insoluble azo pigments such as bench gin yellow, hansa yellow, and lake 4R; lake C, carmine 6B, Bordeaux 10 and the like. Soluble azo pigments;
フタロシアニンブルー、フタロシアニングリーン等の各種(銅)フタロシアニン系顔料;ローダミンレーキ、メチルバイオレットレーキ等の各種の塩素性染め付けレーキ;キノリンレーキ、ファストスカイブルー等の各種の媒染染料系顔料;アンスラキノン系顔料、チオインジゴ系顔料、ペリノン系顔料等の各種の建染染料系顔料;シンカシアレッドB等の各種のキナクリドン系顔料;ヂオキサジンバイオレット等の各種のヂオキサジン系顔料;クロモフタール等の各種の縮合アゾ顔料;アニリンブラックなどが挙げられる。 Various (copper) phthalocyanine pigments such as phthalocyanine blue and phthalocyanine green; various chlorine dyeing lakes such as rhodamine lake and methyl violet lake; various mordant dye pigments such as quinoline lake and fast sky blue; anthraquinone pigment; Various vat dyes such as thioindigo pigments and perinone pigments; various quinacridone pigments such as Cincacia Red B; various dioxazine pigments such as dioxazine violet; various condensed azo pigments such as chromoftal; aniline Black etc. are mentioned.
無機顔料としては、例えば、黄鉛、ジンククロメート、モリブデートオレンジ等の如き、各種のクロム酸塩;紺青等の各種のフェロシアン化合物;酸化チタン、亜鉛華、マピコエロー、酸化鉄、ベンガラ、酸化クロームグリーン、酸化ジルコニウム等の各種の金属酸化物;カドミウムエロー、カドミウムレッド、硫化水銀等の各種の硫化物ないしはセレン化物; Examples of inorganic pigments include various chromates such as chrome lead, zinc chromate, and molybdate orange; various ferrocyan compounds such as bitumen; titanium oxide, zinc white, mapico yellow, iron oxide, bengara, chrome oxide Various metal oxides such as green and zirconium oxide; various sulfides or selenides such as cadmium yellow, cadmium red and mercury sulfide;
硫酸バリウム、硫酸鉛等の各種の硫酸塩;ケイ酸カルシウム、群青等の各種のケイ酸塩;炭酸カルシウム、炭酸マグネシウム等の各種の炭酸塩;コバルトバイオレット、マンガン紫等の各種の燐酸塩;アルミニウム粉、金粉、銀粉、銅粉、ブロンズ粉、真鍮粉等の各種の金属粉末顔料;これら金属のフレーク顔料、マイカ・フレーク顔料;金属酸化物を被覆した形のマイカ・フレーク顔料、雲母状酸化鉄顔料等のメタリック顔料やパール顔料;黒鉛、カーボンブラック等が挙げられる。 Various sulfates such as barium sulfate and lead sulfate; Various silicates such as calcium silicate and ultramarine blue; Various carbonates such as calcium carbonate and magnesium carbonate; Various phosphates such as cobalt violet and manganese purple; Aluminum Various metal powder pigments such as powder, gold powder, silver powder, copper powder, bronze powder and brass powder; flake pigments of these metals, mica flake pigments; mica flake pigments coated with metal oxides, mica-like iron oxide Examples thereof include metallic pigments such as pigments and pearl pigments; graphite and carbon black.
体質顔料としては、例えば、沈降性硫酸バリウム、ご粉、沈降炭酸カルシウム、重炭酸カルシウム、寒水石、アルミナ白、シリカ、含水微粉シリカ(ホワイトカーボン)、超微粉無水シリカ(アエロジル)、珪砂(シリカサンド)、タルク、沈降性炭酸マグネシウム、ベントナイト、クレー、カオリン、黄土などが挙げられる。 Examples of extender pigments include precipitated barium sulfate, powder, precipitated calcium carbonate, calcium bicarbonate, cryolite, alumina white, silica, hydrous finely divided silica (white carbon), ultrafine anhydrous silica (Aerosil), and silica sand (silica). Sand), talc, precipitated magnesium carbonate, bentonite, clay, kaolin, ocher and the like.
さらに、プラスチック顔料としては、例えば、DIC(株)製グランドールPP−1000、PP−2000S等が挙げられる。 Furthermore, examples of the plastic pigment include DIC Corporation Grandol PP-1000, PP-2000S, and the like.
前記の無機充填物類の中でも、紫外線照射試験後の破断強伸度の保持率が、更に向上することから、針状無機充填物以外の無機充填物(例えば、低アスペクト比の無機充填物)、例えば、酸化チタンを併用することが好ましい。 Among the above inorganic fillers, since the retention of breaking strength and elongation after the ultraviolet irradiation test is further improved, inorganic fillers other than acicular inorganic fillers (for example, low aspect ratio inorganic fillers) For example, it is preferable to use titanium oxide in combination.
この場合、針状無機充填物以外の無機充填物100重量部に対して、針状無機充填物を5〜100重量部配合されていることが好ましい。 In this case, it is preferable that 5 to 100 parts by weight of the acicular inorganic filler is blended with 100 parts by weight of the inorganic filler other than the acicular inorganic filler.
本発明の硬化性コーティング組成物、特に上記した主剤には、粘度調整の観点から、そこに含める原料との反応性を有さず、原料を溶解する有機溶剤を含有させることが出来る。具体的には、例えば、トルエン、キシレン等の炭化水素系溶剤、メチルエチルケトン、メチルイソブチルケトン等のケトン系溶剤、酢酸エチル、酢酸ブチル等のエステル系溶剤、ジオキサン、エチレングリコールジエチルエーテル等のエーテル系溶剤、ペンタン、ヘキサン、ヘプタン等の脂肪族系炭化水素等が挙げられる。 From the viewpoint of adjusting the viscosity, the curable coating composition of the present invention, particularly the main component described above, can contain an organic solvent that does not have reactivity with the raw material included therein and dissolves the raw material. Specifically, for example, hydrocarbon solvents such as toluene and xylene, ketone solvents such as methyl ethyl ketone and methyl isobutyl ketone, ester solvents such as ethyl acetate and butyl acetate, ether solvents such as dioxane and ethylene glycol diethyl ether , Aliphatic hydrocarbons such as pentane, hexane and heptane.
本発明の硬化性コーティング組成物には、必要であれば、その他の添加剤などを含有させてもよい。添加剤としては、フィルムやコーティング膜などを形成する樹脂組成物に一般に使用されている添加剤などが挙げられる。添加剤としては、例えば、レベリング剤;コロイド状シリカ、アルミナゾルなどの無機微粒子;ポリメチルメタクリレート系の有機微粒子;消泡剤;タレ性防止剤;シランカップリング剤;粘性調整剤;紫外線吸収剤;金属不活性化剤;過酸化物分解剤;難燃剤;補強剤;可塑剤;潤滑剤;防錆剤;蛍光性増白剤;無機系熱線吸収剤;防炎剤;帯電防止剤;脱水剤;などが挙げられる。 If necessary, the curable coating composition of the present invention may contain other additives. Examples of the additive include additives generally used in resin compositions that form films and coating films. Examples of additives include leveling agents; inorganic fine particles such as colloidal silica and alumina sol; organic fine particles based on polymethyl methacrylate; antifoaming agents; anti-sagging agents; silane coupling agents; viscosity modifiers; Metal deactivator; Peroxide decomposing agent; Flame retardant; Reinforcing agent; Plasticizer; Lubricant; Rust preventive agent; Fluorescent whitening agent; Inorganic heat absorber; Flameproof agent; And so on.
本発明の硬化性コーティング組成物は、通常、硬化剤であるポリイソシアネート化合物以外の各成分をあらかじめ配合した主剤プレミックスを調製しておき、これとポリイソシアネート化合物とを混合して調製することが出来る。 The curable coating composition of the present invention is usually prepared by preparing a main component premix in which components other than the polyisocyanate compound that is a curing agent are blended in advance, and mixing this with the polyisocyanate compound. I can do it.
本発明の硬化性コーティング組成物は、種々の基材に塗布して乾燥することで、基材上に密着性のある硬化塗膜を積層することが出来る。基材への塗布量は、特に制限されるものではないが、例えば、1〜30g/m2、中でも3〜15g/m2の範囲から選択することが、少量で優れた耐候性等が付与できる点で好ましい。この塗布には、例えば、グラビアコーター、マイクログラビアコーター、リバースコーター、バーコーター、ロールコーター、ダイコーター等を用いることが出来る。 The curable coating composition of the present invention can be applied to various substrates and dried to laminate a cured coating film having adhesion on the substrate. The coating amount of the substrate is not particularly limited, for example, 1 to 30 g / m 2, can be selected from a range among them of 3 to 15 g / m 2, excellent weather resistance and the like in small amounts are applied It is preferable in that it can be performed. For this coating, for example, a gravure coater, a micro gravure coater, a reverse coater, a bar coater, a roll coater, a die coater or the like can be used.
また、本発明の硬化性コーティング組成物を塗布した積層体は、作成後エージングを行うことが好ましい。エージング条件は、室温〜100℃で、12〜240時間の間であり、この間に硬化反応が進行する。 Moreover, it is preferable that the laminated body which apply | coated the curable coating composition of this invention performs aging after preparation. The aging conditions are from room temperature to 100 ° C. and for 12 to 240 hours, during which the curing reaction proceeds.
この際の基材としては、例えば、紙、オレフィン系樹脂、アクリロニトリル−ブタジエン−スチレン共重合体(ABS樹脂)、ポリ塩化ビニル系樹脂、フッ素系樹脂、ポリ(メタ)アクリル系樹脂、カーボネート系樹脂、ポリアミド系樹脂、ポリイミド系樹脂、ポリフェニレンエーテル系樹脂、ポリフェニレンスルフィド系樹脂やポリエステル系樹脂から得られた合成樹脂フィルム、銅箔、アルミニウム箔の様な金属箔等を挙げることが出来る。基材の厚みは、特に制限されるものではなく、例えば、10〜400μmから選択出来るが、本発明の硬化性コーティング組成物は、少量の塗布かつ低温短時間の乾燥で、基材に反りやヘタリ等、何ら影響を与えることなく優れた密着性を奏し、優れた耐候性を付与出来ることから、30〜80μmで軟化温度180℃以下の基材への適用が最適である。 Examples of the base material in this case include paper, olefin resin, acrylonitrile-butadiene-styrene copolymer (ABS resin), polyvinyl chloride resin, fluorine resin, poly (meth) acrylic resin, and carbonate resin. And polyamide resin, polyimide resin, polyphenylene ether resin, synthetic resin film obtained from polyphenylene sulfide resin and polyester resin, copper foil, metal foil such as aluminum foil, and the like. The thickness of the substrate is not particularly limited, and can be selected, for example, from 10 to 400 μm. However, the curable coating composition of the present invention can be applied to a substrate with a small amount of application and drying at a low temperature in a short time. Since it exhibits excellent adhesion without giving any influence such as sag and can provide excellent weather resistance, it is most suitable to be applied to a substrate having a softening temperature of 180 ° C. or less at 30 to 80 μm.
低温かつ短時間の乾燥より、基材を反らせたり塗膜剥離したりするなどの不都合が発生することなく、基材への優れた密着性が得られ積層体の劣化をより効果的に防止することが出来る点で、基材としては、ポリエステル樹脂フィルムを用いることが好ましい。本発明の硬化性コーティング組成物の硬化塗膜がポリエステル樹脂フィルム上に積層された、積層ポリエステル樹脂フィルムは、上記した優れた性質を有したものとなる。 Low-temperature and short-time drying eliminates the inconvenience of warping the substrate and peeling the coating film, and provides excellent adhesion to the substrate, preventing deterioration of the laminate more effectively. It is preferable to use a polyester resin film as the base material because it can be used. The laminated polyester resin film in which the cured coating film of the curable coating composition of the present invention is laminated on the polyester resin film has the above-described excellent properties.
特に、160℃以下という比較的低温で1分間以下という短時間の乾燥より、薄膜の基材に上記した様な不都合を発生させず、基材への優れた密着性が得られ積層体の耐湿熱性と耐加水分解性に基づく劣化をより効果的に防止することが出来る点で、基材としては、PETフィルムを用いることがより好ましい。本発明の硬化性コーティング組成物の硬化塗膜がPETフィルム上に積層された、積層ポリエステル樹脂フィルムは、上記した優れた性質を有したものとなる。特に、太陽電池バックシート用の積層ポリエステル樹脂フィルムとして好適である。 In particular, from the drying at a relatively low temperature of 160 ° C. or less for a short time of 1 minute or less, the above-mentioned inconvenience is not caused to the thin film base material, and excellent adhesion to the base material is obtained, and the moisture resistance of the laminated body is obtained. As a base material, it is more preferable to use a PET film in that deterioration based on heat resistance and hydrolysis resistance can be more effectively prevented. The laminated polyester resin film in which the cured coating film of the curable coating composition of the present invention is laminated on the PET film has the above-described excellent properties. In particular, it is suitable as a laminated polyester resin film for a solar battery backsheet.
ポリエステル樹脂フィルムと硬化塗膜との密着性を向上させるために、ポリエステル樹脂フィルムの硬化塗膜を形成する方の面に表面処理を行ってもよい。この表面処理としては、例えば、コロナ処理、プラズマ処理、オゾン処理、火炎処理、放射線処理等が挙げられる。 In order to improve the adhesion between the polyester resin film and the cured coating film, a surface treatment may be performed on the surface on which the cured coating film of the polyester resin film is formed. Examples of the surface treatment include corona treatment, plasma treatment, ozone treatment, flame treatment, and radiation treatment.
本発明の太陽電池モジュールにおいては、透明保護部材、太陽電池用セル、前記太陽電池用セルの全面を覆う封止樹脂、およびバックシートなどの構成は、従来公知の太陽電池モジュールと同様であって、本発明に特有の構成ではない。 In the solar cell module of the present invention, the configuration of the transparent protective member, the solar cell, the sealing resin that covers the entire surface of the solar cell, and the back sheet is the same as that of a conventionally known solar cell module. This is not a configuration specific to the present invention.
すなわち、太陽電池用セルとしては、基板上に透明電極層、光半導体層および裏面電極層を積層し、複数の光電変換セルを形成するように分離溝によって分離され、かつそれらの光電変換セルが電気的に直列接続されてなる集積型太陽電池素子とすることが一般的であり、また、光半導体層中の光電変換層としては、シリコンや薄膜多結晶シリコンなどを用いることができる。さらに、太陽電池用セルからはモジュール外部に電気出力が取り出せるようになっている。 That is, as a cell for solar cells, a transparent electrode layer, an optical semiconductor layer, and a back electrode layer are laminated on a substrate and separated by separation grooves so as to form a plurality of photoelectric conversion cells, and these photoelectric conversion cells are An integrated solar cell element electrically connected in series is generally used, and silicon, thin-film polycrystalline silicon, or the like can be used as the photoelectric conversion layer in the optical semiconductor layer. Furthermore, an electrical output can be taken out of the module from the solar cell.
上記封止樹脂として用いられる樹脂としては、主としてEVAを用いるが、PVB(ポリビニルブチラール)、PIB(ポリイソブチレン)、オレフィン系樹脂(とりわけグラフト変性ポリエチレン樹脂)、アイオノマー樹脂、シリコン樹脂などを用いることもできる。通常、太陽電池モジュールの封止樹脂として用いられるEVAは、酢酸ビニル含有量が10〜40重量%であるものを用い、太陽電池モジュールの耐熱性、物理的強度を確保するために、熱あるいは光などによりEVAを架橋している。 As the resin used as the sealing resin, EVA is mainly used, but PVB (polyvinyl butyral), PIB (polyisobutylene), olefin resin (especially graft-modified polyethylene resin), ionomer resin, silicon resin, etc. may be used. it can. Usually, EVA used as a sealing resin for a solar cell module has a vinyl acetate content of 10 to 40% by weight, and heat or light is used to ensure the heat resistance and physical strength of the solar cell module. EVA is cross-linked by the above.
熱架橋を行う場合は通常有機過酸化物が用いられ、70℃以上の温度で分解してラジカルを発生するものが使用されている。通常、半減期10時間の分解温度が50℃以上のものが用いられ、2,5−ジメチルヘキサン−2,5−ジハイドロキシパーオキサイド、2, 5−ジメチル−2,5−ジ(t−ブチルパーオキシ)ヘキシン−3、ジ−t−ブチルパーオキサイド、t−ブチルクミルパーオキサイド、2,5−ジメチル−2,5−ジ(t−ブチルパーオキシ)ヘキサン、ジクミルパーオキサイド、α,α’−ビス(t−ブチルパーオキシイソプロピル)ベンゼン、n−ブチル−4 ,4−ビス−(t−ブチルパーオキシ)バレレート、t−ブチルパーオキシベンゾエート、ベンゾイルパーオキサイドなどが用いられている。 In the case of performing thermal crosslinking, an organic peroxide is usually used, and one that decomposes at a temperature of 70 ° C. or higher to generate radicals is used. Usually, those having a decomposition temperature of 50 ° C. or more with a half-life of 10 hours are used, and 2,5-dimethylhexane-2,5-dihydroxyperoxide, 2,5-dimethyl-2,5-di (t-butyl) Peroxy) hexyne-3, di-t-butyl peroxide, t-butylcumyl peroxide, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane, dicumyl peroxide, α, α '-Bis (t-butylperoxyisopropyl) benzene, n-butyl-4,4-bis- (t-butylperoxy) valerate, t-butylperoxybenzoate, benzoyl peroxide and the like are used.
光硬化を行う場合には光増感剤が用いられ、水素引き抜き型(二分子反応型)である、ベンゾフェノン、オルソベンゾイル安息香酸メチル、4−ベンゾイル−4'−メチルジフェニルサルファイド、イソプロピルチオキサントンなどが用いられており、内部開裂型開始剤としては、ベンゾインエーテル、ベンジルジメチルケタールなど、α−ヒドロキシアルキルフェノン型として、2−ヒドロキシ−2−メチル−1−フェニルプロパン−1−オン、1−ヒドロキシシクロヘキシルフェニルケトン、アルキルフェニルグリオキシレート、ジエトキシアセトフェノンなどが使用できる。更に、α−アミノアルキルフェノン型として、2−メチル−1−[4(メチルチオ)フェニル]−2−モリフォリノプロパン−1、2−ベンジル−2−ジメチルアミノ−1−(4−モリフォリノフェニル)−ブタノン−1 などが、またアシルフォスフィンオキサイドなども用いられている。 In the case of photocuring, a photosensitizer is used, and hydrogen abstraction type (bimolecular reaction type) such as benzophenone, methyl orthobenzoylbenzoate, 4-benzoyl-4′-methyldiphenyl sulfide, isopropylthioxanthone, etc. As the internal cleavage type initiator, α-hydroxyalkylphenone type such as benzoin ether, benzyldimethyl ketal, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-hydroxycyclohexyl, etc. Phenyl ketone, alkylphenyl glyoxylate, diethoxyacetophenone and the like can be used. Further, as α-aminoalkylphenone type, 2-methyl-1- [4 (methylthio) phenyl] -2-morpholinopropane-1, 2-benzyl-2-dimethylamino-1- (4-morpholino) Phenyl) -butanone-1 and the like, and acylphosphine oxide and the like are also used.
また、太陽電池モジュールを構成するガラス板との接着を考慮してシランカップリング剤も配合されており、ビニルトリエトキシシラン、ビニルトリス(β−メトキシエトキシ)シラン、γ−メタクリロキシプロピルトリメトキシシラン、ビニルトリアセトキシシラン、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、β−(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、γ−クロロプロピルメトキシシラン、ビニルトリクロロシラン、γ−メルカプトプロピルトリメトキシシラン、γ−アミノプロピルトリエトキシシラン、N−β(アミノエチル)−γ−アミノプロピルトリメトキシシランなどが配合されている。 A silane coupling agent is also blended in consideration of adhesion to the glass plate constituting the solar cell module, and vinyltriethoxysilane, vinyltris (β-methoxyethoxy) silane, γ-methacryloxypropyltrimethoxysilane, Vinyltriacetoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, β- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, γ-chloropropylmethoxysilane, vinyltrichlorosilane , Γ-mercaptopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, N-β (aminoethyl) -γ-aminopropyltrimethoxysilane, and the like.
更に、接着性及び硬化を促進する目的でエポキシ基含有化合物を配合されている場合もあり、エポキシ基含有化合物としては、トリグリシジルトリス(2−ヒドロキシエチル)イソシアヌレート、ネオペンチルグリコールジグリシジルエーテル、1,6−ヘキサンジオールジグリシジルエーテル、アクリルグリシジルエーテル、2−エチルヘキシルグリシジルエーテル、フェニルグリシジルエーテル、フェノールグリシジルエーテル、p−t−ブチルフェニルグリシジルエーテル、アジピン酸ジグリシジルエステル、o−フタル酸ジグリシジルエステル、グリシジルメタクリレート、ブチルグリシジルエーテル等の化合物や、エポキシ基を含有した分子量が数百から数千のオリゴマーや重量平均分子量が数千から数十万のポリマーを配合されているケースもある。 Furthermore, an epoxy group-containing compound may be blended for the purpose of promoting adhesion and curing. Examples of the epoxy group-containing compound include triglycidyl tris (2-hydroxyethyl) isocyanurate, neopentyl glycol diglycidyl ether, 1,6-hexanediol diglycidyl ether, acrylic glycidyl ether, 2-ethylhexyl glycidyl ether, phenyl glycidyl ether, phenol glycidyl ether, pt-butylphenyl glycidyl ether, adipic acid diglycidyl ester, o-phthalic acid diglycidyl ester , Glycidyl methacrylate, butyl glycidyl ether and other compounds, oligomers containing an epoxy group with a molecular weight of several hundred to several thousand, and polymers with a weight average molecular weight of several thousand to several hundred thousand. Some cases are there.
そしてさらに、封止樹脂の架橋、接着性、機械的強度、耐熱性、耐湿熱性、耐候性などを向上させ目的で、アクリロキシ基、メタクリロキシ基又はアリル基含有化合物を添加されており、(メタ)アクリル酸誘導体、例えばそのアルキルエステルやアミドが最も一般的である。この場合、アルキル基としては、メチル、エチル、ドデシル、ステアリル、ラウリルのようなアルキル基の他に、シクロヘキシル基、テトラヒドロフルフリル基、アミノエチル基、2−ヒドロキシエチル基、3−ヒドロキシプロピル基、3−クロロ−2−ヒドロキシプロピル基などが挙げられる。また、(メタ)アクリル酸とエチレングリコール、トリエチレングリコール、ポリエチレングリコール、グリセリン、トリメチロールプロパン、ペンタエリスリトール等の多官能アルコールとのエステルも同様に用いられる。アミドとしては、アクリルアミドが代表的である。また、アリル基含有化合物としては、トリ
アリルシアヌレート、トリアリルイソシアヌレート、フタル酸ジアリル、イソフタル酸ジアリル、マレイン酸ジアリル等が配合されている。
Further, an acryloxy group, methacryloxy group or allyl group-containing compound is added for the purpose of improving the crosslinking resin, adhesion, mechanical strength, heat resistance, heat and humidity resistance, weather resistance, etc. Acrylic acid derivatives such as their alkyl esters and amides are most common. In this case, as the alkyl group, in addition to an alkyl group such as methyl, ethyl, dodecyl, stearyl, lauryl, cyclohexyl group, tetrahydrofurfuryl group, aminoethyl group, 2-hydroxyethyl group, 3-hydroxypropyl group, A 3-chloro-2-hydroxypropyl group and the like can be mentioned. Further, esters of (meth) acrylic acid and polyfunctional alcohols such as ethylene glycol, triethylene glycol, polyethylene glycol, glycerin, trimethylolpropane, pentaerythritol and the like are also used. A typical amide is acrylamide. Further, as the allyl group-containing compound, triallyl cyanurate, triallyl isocyanurate, diallyl phthalate, diallyl isophthalate, diallyl maleate and the like are blended.
さらには、難燃性を付与するための無機化合物や、耐候性を付与するための紫外線吸収剤、酸化劣化防止のための酸化防止剤も種々に配合されている。つまり、太陽電池モジュールを構成するEVAは、太陽電池モジュールとして要求される機能を満たすべく、各種添加剤を配合した樹脂組成物である。 Furthermore, an inorganic compound for imparting flame retardancy, an ultraviolet absorber for imparting weather resistance, and an antioxidant for preventing oxidative degradation are variously blended. That is, EVA which comprises a solar cell module is a resin composition which mix | blended various additives in order to satisfy | fill the function requested | required as a solar cell module.
太陽電池モジュールとして一体化する方法について、その一例として、真空ラミネート方式が挙げられる。この方法は、例えば、100〜150℃に加熱された真空ラミネート装置の加熱板上のダミーガラスや金属板の上に、透明保護部材、透明保護部材側の封止樹脂、配線を施した太陽電池用セル、バックシート側の封止樹脂、およびバックシートの順に積層して、静置する。その後、真空ラミネート装置を閉じて減圧を開始し、この減圧状態を3〜10分間保持した後、給排気管から空気を導入して、圧力差によりゴム製ダイアフラムを上記積層体に押し当て加圧する。封止樹脂の種類にもよるが、この状態を10〜40分間保持することで加熱真空ラミネート工程が完了する。 As an example of a method for integrating as a solar cell module, a vacuum laminating method can be given. This method is, for example, a solar cell in which a transparent protective member, a sealing resin on the transparent protective member side, and a wiring are provided on a dummy glass or a metal plate on a heating plate of a vacuum laminating apparatus heated to 100 to 150 ° C. The cell, the back sheet side sealing resin, and the back sheet are laminated in this order and allowed to stand. Thereafter, the vacuum laminating apparatus is closed and pressure reduction is started. After this pressure reduction state is maintained for 3 to 10 minutes, air is introduced from the air supply / exhaust pipe, and the rubber diaphragm is pressed against the laminated body by pressure difference to pressurize. . Although depending on the type of sealing resin, the heated vacuum laminating step is completed by holding this state for 10 to 40 minutes.
また、上記真空ラミネート方式は、一例に過ぎず、公知のラミネート方式を適用することができる。 Moreover, the said vacuum laminating system is only an example, and a well-known laminating system can be applied.
上記のとおり、本発明の硬化性コーティング組成物をポリエステル樹脂フィルム上に積層した積層ポリエステル樹脂フィルムをバックシートとして用いると、従来の硬化性コーティング組成物と比較して、耐光性、ポリエステル樹脂フィルムとの密着性、及び高温高湿試験後のポリエステル樹脂フィルムとの密着性が格段に向上する。更に、EVA等の封止樹脂への接着性、耐加水分解性、耐ブロッキング性に優れた性能を発揮することができる。 As described above, when a laminated polyester resin film obtained by laminating the curable coating composition of the present invention on a polyester resin film is used as a back sheet, light resistance, polyester resin film and And the adhesion to the polyester resin film after the high temperature and high humidity test are significantly improved. Furthermore, performance excellent in adhesion to sealing resins such as EVA, hydrolysis resistance, and blocking resistance can be exhibited.
以下に、実施例を用いて本発明を具体的に説明する。尚、実施例中の「部」は、重量基準である。 Hereinafter, the present invention will be specifically described with reference to examples. In the examples, “part” is based on weight.
本発明に用いる水酸基を含有する樹脂(A)の数平均分子量は、ゲルパーミッションクロマトグラフ(GPC)を用い、下記の条件により求めた。
測定装置;東ソー株式会社製 HLC−8220
検出器;RI(示差屈折計)
測定条件;カラム温度 40℃ 溶媒 テトラヒドロフラン
また、本発明に用いる水酸基を含有する樹脂(A)のガラス転移温度は、下記の条件により求めた。
The number average molecular weight of the hydroxyl group-containing resin (A) used in the present invention was determined under the following conditions using a gel permeation chromatograph (GPC).
Measuring device: HLC-8220 manufactured by Tosoh Corporation
Detector: RI (differential refractometer)
Measurement conditions: Column temperature 40 ° C. Solvent tetrahydrofuran The glass transition temperature of the hydroxyl group-containing resin (A) used in the present invention was determined under the following conditions.
測定装置;セイコー電子工業株式会社製 DSC220C
測定方法;DSC(示差走査熱量分析)法
Measuring device: DSC220C manufactured by Seiko Electronics Corporation
Measuring method: DSC (Differential Scanning Calorimetry) method
実施例1〜6
下記の表1−1、及び表1−2に示す通り、水酸基を含有する樹脂(A)、ポリイソシアネート化合物(B)、針状無機充填物、針状無機充填物以外の無機充填物を用いて、主剤成分と硬化剤成分との二液型の、本発明の硬化性コーティング組成物を調製した。
実施例7
下記の表1−2に示す通り、水酸基を含有する樹脂(A)、ポリイソシアネート化合物(B)、針状無機充填物を用いて、主剤成分と硬化剤成分との二液型の、本発明の硬化性コーティング組成物を調製した。
比較例1〜4
下記の表2−1、及び表2−2に示す通り、水酸基を含有する樹脂(A)、ポリイソシアネート化合物(B)、針状無機充填物以外の無機充填物を用いて、主剤成分と硬化剤成分との二液型の、従来の硬化性コーティング組成物を調製した。
比較例5
下記の表2−2に示す通り、水酸基を含有する樹脂(A)、ポリイソシアネート化合物(B)、針状無機充填物以外の無機充填物、エポキシ樹脂を用いて、主剤成分と硬化剤成分との二液型の、従来の硬化性コーティング組成物を調製した。
比較例6
下記の表2−2に示す通り、水酸基を含有する樹脂(A)、ポリイソシアネート化合物(B)、針状無機充填物以外の無機充填物、エポキシ樹脂、紫外線吸収剤を用いて、主剤成分と硬化剤成分との二液型の、従来の硬化性コーティング組成物を調製した。
Examples 1-6
As shown in the following Table 1-1 and Table 1-2, an inorganic filler other than the hydroxyl group-containing resin (A), polyisocyanate compound (B), acicular inorganic filler, and acicular inorganic filler is used. Thus, a two-pack type curable coating composition of the present invention comprising a main component and a curing agent component was prepared.
Example 7
As shown in Table 1-2 below, the present invention is a two-pack type of a main component and a curing agent component using a resin (A) containing a hydroxyl group, a polyisocyanate compound (B), and an acicular inorganic filler. A curable coating composition was prepared.
Comparative Examples 1-4
As shown in Table 2-1 and Table 2-2 below, the main ingredient component and curing are performed using an inorganic filler other than the hydroxyl group-containing resin (A), polyisocyanate compound (B), and acicular inorganic filler. A conventional two-part curable coating composition with an agent component was prepared.
Comparative Example 5
As shown in Table 2-2 below, using a resin (A) containing a hydroxyl group, a polyisocyanate compound (B), an inorganic filler other than an acicular inorganic filler, and an epoxy resin, A conventional two-part curable coating composition was prepared.
Comparative Example 6
As shown in Table 2-2 below, the main component component and the resin containing a hydroxyl group (A), polyisocyanate compound (B), inorganic filler other than needle-like inorganic filler, epoxy resin, and ultraviolet absorber A conventional two-part curable coating composition with a hardener component was prepared.
前記硬化性コーティング組成物を乾燥後の塗工量が10g/m2となるように「E5001」(東洋紡(株)製 PETフィルム)に塗布し、80℃、30秒間乾燥させ、硬化塗膜を形成した後、40℃で3日間エージングを行なった。また、「E5001」の代わりに「X10S」(東レ(株)製 耐侯性PET)を用いた場合についても、同様に塗工物を作成した。 The curable coating composition is applied to “E5001” (PET film manufactured by Toyobo Co., Ltd.) so that the coating amount after drying is 10 g / m 2 and dried at 80 ° C. for 30 seconds to form a cured coating film. Then, aging was performed at 40 ° C. for 3 days. Moreover, the coated material was similarly created also when using "X10S" (Toray Industries, Inc. weather-resistant PET) instead of "E5001".
(PETフィルムとの密着性評価サンプルの作製方法)
前記硬化性コーティング組成物を設けた塗工物を幅100mm、長さ250mmに裁断して、温度120℃、相対湿度100%RHの環境条件で、48時間や72時間のプレッシャークッカー試験(以下、PCT試験という)を行った。
(Method for producing sample for evaluating adhesion to PET film)
The coated product provided with the curable coating composition is cut into a width of 100 mm and a length of 250 mm, and a pressure cooker test (hereinafter, referred to as 48 hours or 72 hours under an environmental condition of a temperature of 120 ° C. and a relative humidity of 100% RH). PCT test).
(PETフィルムとの密着性の評価方法)
前記硬化性コーティング組成物を設けた塗工物について、PCT試験をしなかったもの(初期)、試験をしたもの(湿熱経時後)をJIS5600−5−6クロスカット法に従い、硬化性コーティング組成物とPETフィルム基材の剥離を測定した。
尚、表1−1,1−2,2−1,2−2中の密着性条件(1)、(2)は以下のものとする。
密着性条件(1):PCT 120℃、100%RH、48時間、基材:E5001(東洋紡株式会社汎用PETフィルム)
密着性条件(2):PCT 120℃、100%RH、76時間、基材:X10S (東レ株式会社耐侯PETフィルム)
(Evaluation method for adhesion to PET film)
About the coated material provided with the curable coating composition, the one that was not subjected to the PCT test (initial) and the one that was tested (after wet heat aging) were curable according to JIS 5600-5-6 cross-cut method. And the peeling of the PET film substrate was measured.
The adhesion conditions (1) and (2) in Tables 1-1, 1-2, 2-1 and 2-2 are as follows.
Adhesion condition (1): PCT 120 ° C., 100% RH, 48 hours, substrate: E5001 (Toyobo Co., Ltd. general-purpose PET film)
Adhesion condition (2): PCT 120 ° C., 100% RH, 76 hours, substrate: X10S (Toray Industries, Inc. PET-resistant film)
(紫外線照射試験後の破断強伸度維持の評価方法)
前記硬化性コーティング組成物を設けた塗工物について、アイスーパーUVテスターSUV−W161(岩崎電気株式会社製)で、UV照度100mW/cm2、100時間照射して、株式会社エー・アンド・ディー製テンシロン万能材料試験機にて破断強伸度を測定した。
尚、PCT前後における各強度の保持率が、90%以上を◎、89〜80%を○、79〜70%を△、69%以下を×とした。
(Evaluation method for maintaining strength at break after UV irradiation test)
The coated product provided with the curable coating composition was irradiated with an i-super UV tester SUV-W161 (manufactured by Iwasaki Electric Co., Ltd.) for 100 hours with UV illuminance of 100 mW / cm 2 , and A & D Co., Ltd. The tensile strength at break was measured with a Tensilon universal material testing machine.
In addition, the retention rate of each strength before and after PCT is 90% or more as ◎, 89 to 80% as ○, 79 to 70% as Δ, and 69% or less as ×.
なお、前記表中の材料の概要を下記に示す。
エリーテルUE−3210:ポリエステル樹脂(ユニチカ株式会社)、固形分:100%
Tg:45℃、水酸基価:4mgKOH/g、数平均分子量:20,000、固形分:50%、Tg:70℃、水酸基価:20
アクリディックA−808:水酸基含有アクリル樹脂(DIC株式会社)、固形分:50%、Tg:41℃、水酸基価:40
アクリディックA−809:水酸基含有アクリル樹脂(DIC株式会社)、固形分:50%、Tg:41℃、水酸基価:20
フルオネートK−704 :フッ素含有ポリオール樹脂(DIC株式会社)、固形分:60%、Tg:41℃、水酸基価:40
エピクロン860:ビスフェノールA型エポキシ樹脂(DIC株式会社)、固形分:100%、エポキシ当量:240
チヌビン479:紫外線吸収剤(BASFジャパン株式会社)固形分:100%
JR−805:酸化チタン(テイカ株式会社)アスペクト比:1〜2
ティスモD101:チタン酸カリウムウィスカ(大塚化学株式会社)アスペクト比:15〜100
SH−1800:ウォラストナイトウィスカ(キンセイマテック株式会社)アスペクト比:10〜20
FTL−100:針状酸化チタン(テイカ株式会社)アスペクト比:13(代表値)
スミジュールN3300:HDI系ポリイソシアネート(住化バイエルウレタン株式会社)固形分:100%
The outline of the materials in the table is shown below.
Elitel UE-3210: Polyester resin (Unitika Ltd.), solid content: 100%
Tg: 45 ° C., hydroxyl value: 4 mg KOH / g, number average molecular weight: 20,000, solid content: 50%, Tg: 70 ° C., hydroxyl value: 20
Acrydic A-808: hydroxyl group-containing acrylic resin (DIC Corporation), solid content: 50%, Tg: 41 ° C., hydroxyl value: 40
Acrydic A-809: hydroxyl group-containing acrylic resin (DIC Corporation), solid content: 50%, Tg: 41 ° C., hydroxyl value: 20
Fluorate K-704: Fluorine-containing polyol resin (DIC Corporation), solid content: 60%, Tg: 41 ° C., hydroxyl value: 40
Epicron 860: Bisphenol A type epoxy resin (DIC Corporation), solid content: 100%, epoxy equivalent: 240
Tinuvin 479: UV absorber (BASF Japan Ltd.) Solid content: 100%
JR-805: Titanium oxide (Taika Corporation) Aspect ratio: 1-2
Tismo D101: Potassium titanate whisker (Otsuka Chemical Co., Ltd.) Aspect ratio: 15-100
SH-1800: Wollastonite whisker (Kinsei Matec Corporation) Aspect ratio: 10-20
FTL-100: Acicular titanium oxide (Taika Corporation) Aspect ratio: 13 (representative value)
Sumidur N3300: HDI polyisocyanate (Sumika Bayer Urethane Co., Ltd.) Solid content: 100%
本発明の硬化性コーティング組成物は、より優れた耐光性、密着性、耐候性を有するので、例えば鉄道車両、自動車、自動販売機等の表面に貼付して用いられるマーキング用フィルムの表面保護、光沢向上、変退色・劣化防止等を目的としたオーバーレイフィルムや、車両や住宅のプラスチック製ウインドウや外装看板の表面保護用フィルム、液晶ディスプレイ反射用シート、太陽電池用バックシート等として、主として精密部品の保護や変退色防止の目的で用いられる高耐候性フィルム・シートを提供出来る。 Since the curable coating composition of the present invention has more excellent light resistance, adhesion, and weather resistance, for example, surface protection of a marking film used by being attached to the surface of a railway vehicle, automobile, vending machine, etc. Precision parts mainly as overlay films for improving gloss, preventing discoloration / deterioration, etc., surface protection films for plastic windows and exterior signs for vehicles and houses, LCD sheet reflective sheets, solar cell back sheets, etc. It is possible to provide a highly weather-resistant film and sheet used for the purpose of protecting the color and preventing discoloration.
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