JP5075849B2 - 透明複合材料 - Google Patents
透明複合材料 Download PDFInfo
- Publication number
- JP5075849B2 JP5075849B2 JP2009017448A JP2009017448A JP5075849B2 JP 5075849 B2 JP5075849 B2 JP 5075849B2 JP 2009017448 A JP2009017448 A JP 2009017448A JP 2009017448 A JP2009017448 A JP 2009017448A JP 5075849 B2 JP5075849 B2 JP 5075849B2
- Authority
- JP
- Japan
- Prior art keywords
- composite material
- vinyl ester
- transparent composite
- ester resin
- mass
- 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.)
- Expired - Fee Related
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 229910021647 smectite Inorganic materials 0.000 claims abstract description 83
- 229920001567 vinyl ester resin Polymers 0.000 claims abstract description 59
- 229920005989 resin Polymers 0.000 claims abstract description 56
- 239000011347 resin Substances 0.000 claims abstract description 56
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 239000011342 resin composition Substances 0.000 claims abstract description 29
- 150000001875 compounds Chemical class 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 20
- 238000010894 electron beam technology Methods 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000004593 Epoxy Substances 0.000 claims abstract description 16
- 150000004714 phosphonium salts Chemical group 0.000 claims abstract description 12
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- -1 glycidyl compound Chemical class 0.000 claims description 51
- 239000002904 solvent Substances 0.000 claims description 38
- 238000001723 curing Methods 0.000 claims description 29
- 239000000178 monomer Substances 0.000 claims description 21
- 150000003839 salts Chemical class 0.000 claims description 19
- 238000002834 transmittance Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 11
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 9
- 238000013007 heat curing Methods 0.000 claims description 9
- 239000003822 epoxy resin Substances 0.000 claims description 8
- 229920000647 polyepoxide Polymers 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 125000002723 alicyclic group Chemical group 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 239000004973 liquid crystal related substance Substances 0.000 claims description 5
- AZJYLVAUMGUUBL-UHFFFAOYSA-A u1qj22mc8e Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[F-].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O=[Si]=O.O=[Si]=O.O=[Si]=O.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 AZJYLVAUMGUUBL-UHFFFAOYSA-A 0.000 claims description 5
- OGQYPPBGSLZBEG-UHFFFAOYSA-N dimethyl(dioctadecyl)azanium Chemical class CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC OGQYPPBGSLZBEG-UHFFFAOYSA-N 0.000 claims description 4
- ZUZLIXGTXQBUDC-UHFFFAOYSA-N methyltrioctylammonium Chemical class CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC ZUZLIXGTXQBUDC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000275 saponite Inorganic materials 0.000 claims description 4
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical class CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- NDMVEPBCXVVMEN-UHFFFAOYSA-N dibenzyl(dioctadecyl)azanium Chemical compound C=1C=CC=CC=1C[N+](CCCCCCCCCCCCCCCCCC)(CCCCCCCCCCCCCCCCCC)CC1=CC=CC=C1 NDMVEPBCXVVMEN-UHFFFAOYSA-N 0.000 claims description 3
- VICYBMUVWHJEFT-UHFFFAOYSA-N dodecyltrimethylammonium ion Chemical group CCCCCCCCCCCC[N+](C)(C)C VICYBMUVWHJEFT-UHFFFAOYSA-N 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- 239000003760 tallow Substances 0.000 claims description 3
- PDSVZUAJOIQXRK-UHFFFAOYSA-N trimethyl(octadecyl)azanium Chemical class CCCCCCCCCCCCCCCCCC[N+](C)(C)C PDSVZUAJOIQXRK-UHFFFAOYSA-N 0.000 claims description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 60
- 238000000034 method Methods 0.000 description 35
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 16
- 239000006185 dispersion Substances 0.000 description 15
- 238000000576 coating method Methods 0.000 description 13
- 239000011521 glass Substances 0.000 description 12
- 238000003848 UV Light-Curing Methods 0.000 description 10
- 239000003963 antioxidant agent Substances 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 239000010410 layer Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000005341 cation exchange Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 239000000314 lubricant Substances 0.000 description 7
- 229920003023 plastic Polymers 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 239000006096 absorbing agent Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 238000002296 dynamic light scattering Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 125000003827 glycol group Chemical group 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 4
- 239000012965 benzophenone Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 4
- 239000002985 plastic film Substances 0.000 description 4
- 229920006255 plastic film Polymers 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 3
- XOUQAVYLRNOXDO-UHFFFAOYSA-N 2-tert-butyl-5-methylphenol Chemical compound CC1=CC=C(C(C)(C)C)C(O)=C1 XOUQAVYLRNOXDO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000003093 cationic surfactant Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- 229920001451 polypropylene glycol Polymers 0.000 description 3
- 239000001294 propane Substances 0.000 description 3
- 239000007870 radical polymerization initiator Substances 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 2
- BVUXDWXKPROUDO-UHFFFAOYSA-N 2,6-di-tert-butyl-4-ethylphenol Chemical compound CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 BVUXDWXKPROUDO-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 229920001651 Cyanoacrylate Polymers 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- MWCLLHOVUTZFKS-UHFFFAOYSA-N Methyl cyanoacrylate Chemical compound COC(=O)C(=C)C#N MWCLLHOVUTZFKS-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000003570 air Substances 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 2
- 239000012964 benzotriazole Substances 0.000 description 2
- USFRYJRPHFMVBZ-UHFFFAOYSA-M benzyl(triphenyl)phosphanium;chloride Chemical compound [Cl-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)CC1=CC=CC=C1 USFRYJRPHFMVBZ-UHFFFAOYSA-M 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000007809 chemical reaction catalyst Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001227 electron beam curing Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- SFLRURCEBYIKSS-UHFFFAOYSA-N n-butyl-2-[[1-(butylamino)-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound CCCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCCC SFLRURCEBYIKSS-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 150000001451 organic peroxides Chemical class 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000003505 polymerization initiator Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- ODLMAHJVESYWTB-UHFFFAOYSA-N propylbenzene Chemical compound CCCC1=CC=CC=C1 ODLMAHJVESYWTB-UHFFFAOYSA-N 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000007142 ring opening reaction Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 description 2
- 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 2
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 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 1
- KYLUAQBYONVMCP-UHFFFAOYSA-N (2-methylphenyl)phosphane Chemical compound CC1=CC=CC=C1P KYLUAQBYONVMCP-UHFFFAOYSA-N 0.000 description 1
- FVQMJJQUGGVLEP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOOC(C)(C)C FVQMJJQUGGVLEP-UHFFFAOYSA-N 0.000 description 1
- HCXVPNKIBYLBIT-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 3,5,5-trimethylhexaneperoxoate Chemical compound CC(C)(C)CC(C)CC(=O)OOOC(C)(C)C HCXVPNKIBYLBIT-UHFFFAOYSA-N 0.000 description 1
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
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- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- YPVDWEHVCUBACK-UHFFFAOYSA-N propoxycarbonyloxy propyl carbonate Chemical compound CCCOC(=O)OOC(=O)OCCC YPVDWEHVCUBACK-UHFFFAOYSA-N 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 229920005612 synthetic inorganic polymer Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- VNJISVYSDHJQFR-UHFFFAOYSA-N tert-butyl 4,4-dimethylpentaneperoxoate Chemical compound CC(C)(C)CCC(=O)OOC(C)(C)C VNJISVYSDHJQFR-UHFFFAOYSA-N 0.000 description 1
- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- LVEOKSIILWWVEO-UHFFFAOYSA-N tetradecyl 3-(3-oxo-3-tetradecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCC LVEOKSIILWWVEO-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical compound [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 description 1
- BRKFQVAOMSWFDU-UHFFFAOYSA-M tetraphenylphosphanium;bromide Chemical compound [Br-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 BRKFQVAOMSWFDU-UHFFFAOYSA-M 0.000 description 1
- WAGFXJQAIZNSEQ-UHFFFAOYSA-M tetraphenylphosphonium chloride Chemical compound [Cl-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 WAGFXJQAIZNSEQ-UHFFFAOYSA-M 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- WLPUWLXVBWGYMZ-UHFFFAOYSA-N tricyclohexylphosphine Chemical compound C1CCCCC1P(C1CCCCC1)C1CCCCC1 WLPUWLXVBWGYMZ-UHFFFAOYSA-N 0.000 description 1
- MZHULIWXRDLGRR-UHFFFAOYSA-N tridecyl 3-(3-oxo-3-tridecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCC MZHULIWXRDLGRR-UHFFFAOYSA-N 0.000 description 1
- WUMSTCDLAYQDNO-UHFFFAOYSA-N triethoxy(hexyl)silane Chemical compound CCCCCC[Si](OCC)(OCC)OCC WUMSTCDLAYQDNO-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- FZMJEGJVKFTGMU-UHFFFAOYSA-N triethoxy(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC FZMJEGJVKFTGMU-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- IKANSXQHJXBNIN-UHFFFAOYSA-N trimethyl(octadecyl)phosphanium Chemical class CCCCCCCCCCCCCCCCCC[P+](C)(C)C IKANSXQHJXBNIN-UHFFFAOYSA-N 0.000 description 1
- ZNEOHLHCKGUAEB-UHFFFAOYSA-N trimethylphenylammonium Chemical compound C[N+](C)(C)C1=CC=CC=C1 ZNEOHLHCKGUAEB-UHFFFAOYSA-N 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/036—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes
- H01L31/0392—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/036—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes
- H01L31/0392—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
- H01L31/03926—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate comprising a flexible substrate
-
- 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
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Liquid Crystal (AREA)
- Electroluminescent Light Sources (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Polymerisation Methods In General (AREA)
- Epoxy Resins (AREA)
Description
2.前記ビニルエステル樹脂が、脂環式構造を有するエポキシ化合物から合成されるビニルエステル樹脂である前記1に記載の透明複合材料。
3.前記ビニルエステル樹脂が、水素化ビスフェノールA型エポキシ樹脂から合成されるビニルエステル樹脂である前記1または2に記載の透明複合材料。
4.前記ビニルエステル樹脂組成物が、ビニルエステル樹脂30質量%〜100質量%とエチレン性不飽和基を有する反応性モノマー0質量%〜70質量%とから構成される前記1〜3のいずれかに記載の透明複合材料。
5.前記合成スメクタイトが、合成ヘクトライト、合成サポナイト、及び合成スティーブンサイトから選択される1種以上である前記1に記載の透明複合材料。
6.前記合成スメクタイトを有機化処理するための4級アンモニウム塩が、ラウリルトリメチルアンモニウム塩、ステアリルトリメチルアンモニウム塩、トリオクチルメチルアンモニウム塩、ジステアリルジメチルアンモニウム塩、ジ硬化牛脂ジメチルアンモニウム塩、ジステアリルジベンジルアンモニウム塩、及びN−ポリオキシエチレン−N−ラウリル−N,N−ジメチルアンモニウム塩の1種以上から選択される前記1に記載の透明複合材料。
7.合成スメクタイトの表面に存在する水酸基が、表面改質剤によって処理されたものである前記1、5または6に記載の透明複合材料。
8.前記表面改質剤が、シランカップリング剤、チタネートカップリング剤、グリシジル化合物、イソシアネート化合物、カルボン酸類、及びアルコール類から選択されるものである前記7に記載の透明複合材料。
9.50℃〜250℃での面方向の平均線膨張係数が30ppm/℃以下で、かつ100μm厚当たりでの全光線透過率が85%以上である前記1〜8のいずれかに記載の透明複合材料からなる透明板。
10.硬化前のビニルエステル樹脂組成物、合成スメクタイト、及び溶剤を含む組成物を、表面が平滑な平面上に塗布した後、溶剤を乾燥し、表面が平滑なシートまたはフィルムで挟み、電子線(EB)、紫外線(UV)または熱硬化させる前記1〜8のいずれかに記載の透明複合材料の製造方法。
11.前記1〜8のいずれかに記載の透明複合材料を基材とした表示装置。
12.前記表示装置が、液晶ディスプレイ、有機ELディスプレイ、または電子ペーパーである前記11に記載の表示装置。
13.前記1〜8のいずれかに記載の透明複合材料を基材とした太陽電池用基板。
従来、樹脂の透明性を維持したまま、機械特性及び熱特性を改善することができるフィラーとしては、ガラスクロスやナノシリカ等が知られている。しかし、ガラスクロスの場合には、樹脂とガラスクロスとの線膨張係数が大きく異なるために、加熱・冷却時のマイクロクラックにより白化し材料の透明性が失われる。また、ナノシリカを充填した場合には、少量の添加では透明性は維持できるものの、ディスプレイ基板や太陽電池用基板の用途に要求される低線膨張係数を達成するためにはナノシリカを高充填する必要があり、この場合には透明性を維持することはできない。また、ベントナイト等の天然クレイを充填する場合には、機械物性、熱物性の向上を図ることが可能であるが、天然クレイ結晶内の酸化鉄やクオーツ等の不純物を完全に除去することは不可能であり、機械特性、熱特性、透明性の向上の実現は困難である。本発明における透明複合材料は、特定の性状を有する合成スメクタイトが分散している、脂肪族エポキシ化合物から合成されるビニルエステル樹脂を含むビニルエステル樹脂組成物の50℃〜250℃での面方向の平均線膨張係数が30ppm/℃以下である透明複合材料である。
本発明におけるビニルエステル樹脂とは、エポキシ(メタ)アクリレートとも呼ばれ、一般に(1)エポキシ樹脂に代表されるエポキシ化合物と、(メタ)アクリル酸等のラジカル重合性の炭素−炭素二重結合(エチレン性不飽和基)を有するカルボキシル化合物のカルボキシル基との開環反応により合成されるエチレン性不飽和基を有する樹脂、または(2)カルボキシル基を持つ化合物と、グリシジル(メタ)アクリレート等の分子内にエポキシ基を持つ重合性不飽和化合物のエポキシ基との開環反応により合成される重合性不飽和基を有する樹脂を指す。詳しくは「ポリエステル樹脂ハンドブック」,日刊工業新聞社,1988年発行,第336頁〜357頁などに記載されている。このビニルエステル樹脂は公知の方法により製造することができる。また、本発明において、ビニルエステル樹脂組成物とは、ビニルエステル樹脂と反応性モノマーを含む組成物をいう。
本発明のビニルエステル樹脂組成物には、硬化速度のコントロール、粘度調整(作業性の改善)、架橋密度の向上、機能付加等を目的として反応性モノマーを加えることもできる。これらの反応性モノマーとしては特に制限はなく、種々のものが使用できるが、ビニルエステル樹脂組成物と反応させるためにはビニル基、アリル基等のラジカル重合性の炭素−炭素二重結合(エチレン性不飽和基)を有するモノマーが好ましい。このようなモノマーとして一分子中に一個のエチレン性不飽和基を有する単官能モノマー、一分子中に二個以上のエチレン性不飽和基を有する多官能モノマーが挙げられる。これら反応性モノマーの好ましい具体例を以下に示す。
本発明に用いられる合成スメクタイトは、数平均粒径が10nm〜300nmであり、アスペクト比が10〜300である合成スメクタイトであれば特に限定されない。
さらに、表面改質剤を用いることによりビニルエステル樹脂中に合成スメクタイトを高度に分散させることができる。どのような、表面改質剤を用いれば分散性が向上するかは、一般的に脂肪族炭素鎖を多く含むビニルエステル樹脂には脂肪族系の、表面改質剤を用いるのが好ましい。
本発明のビニルエステル樹脂組成物を硬化させる場合には電子線(EB)硬化が好ましいが、紫外線(UV)または熱硬化することも可能である。UVまたは熱硬化させる場合には、硬化剤を使用してもよい。使用できる硬化剤としては特に制限はなく、一般に重合性樹脂の硬化剤として用いられているものを用いることができる。中でも、(メタ)アクリロイルオキシ基の重合開始の点からラジカル重合開始剤を添加することが望ましい。ラジカル重合開始剤としては、光重合開始剤、有機過酸化物、アゾ化合物等が挙げられる。本発明のビニルエステル樹脂組成物をUV硬化させる点からは光重合開始剤が特に好ましい。
本発明の透明導電性基板用ビニルエステル樹脂組成物には、硬度、強度、成形性、耐久性、耐水性を改良する目的で、紫外線吸収剤、酸化防止剤、消泡剤、レベリング剤、離型剤、滑剤、撥水剤、難燃剤、低収縮剤、架橋助剤などの添加剤を必要に応じて添加することができる。
本発明において合成スメクタイトを効率的に層剥離させ、ビニルエステル樹脂組成物中に分散させるために溶剤を使用することが好ましい。溶剤としては、例えばベンゼン、トルエン、キシレン、エチルベンゼン、メシチレン、n−プロピルベンゼン、イソプロピルベンゼン等の芳香族炭化水素類、酢酸メチル、酢酸エチル、酢酸プロピル、酢酸ブチル等の酢酸エステル類、アセトン、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類、ジエチルエーテル、テトラヒドロフラン、1,4−ジオキサン等のエーテル類、メタノール、エタノール、(イソ)プロパノール、ブチルアルコール等のアルコール類、クロロホルム、塩化メチレン等のハロゲン化炭化水素類、N,N−ジメチルホルムアミド、N−メチルピロリドン、ピリジン、アセトニトリル等の含窒素系溶剤等が挙げられる。好ましくは、操作性の観点から水、メタノール等のアルコール類、トルエン、キシレン、N−メチルピロリドンが挙げられる。
本発明の透明シートは、4級アンモニウム及び/または4級ホスホニウムによって有機化処理された合成スメクタイト、ビニルエステル樹脂組成物の混合物を基材上に塗布し、EB/UVまたは熱硬化し、得られた透明シートを剥離して製造することができる。
柔軟性は、2mmφのガラス棒に作成したフィルムを巻きつけて評価した。巻きつけることができる場合を○、できない場合を×とした。
線膨張係数は、エスアイアイ・ナノテクノロジー社製TMA/SS6100を使用し、引張モードで測定を行った。フィルム状試験片は、厚さ100μm×3mm×12mm(チャック間距離10mm)、張力:0.001kgfとし、窒素を100mL/minの雰囲気下で昇温速度5℃/minで250℃まで温度を上げた後、50℃以下まで冷却し、再度、昇温速度5℃/minで50℃〜250℃までの間で、試験片の伸長率を測定した。50℃と250℃との伸長率差と温度差(200℃)とから50℃〜250℃の間の面方向の平均線膨張係数を計算した。また、伸長率の不連続点の温度をガラス転移温度(Tg)とした。
全光線透過率は、東京電色社製全自動ヘーズメーターTC−H3DPKを使用し、JIS K−7361−1に準拠して測定した。
ヘーズ値は、東京電色社製全自動ヘーズメーターTC−H3DPKを使用し、JIS K−7136に準拠して測定した。
温度調節器、撹拌装置、ジムロート冷却管、空気導入管を付した四つ口フラスコに、東都化成社製水添ビスフェノールA型エポキシ樹脂 ST−4000D(商品名、エポキシ当量:725)276.3部(質量部,以下同じ)、トルエン202.5部、重合禁止剤として4−メトキシフェノール(MEHQ:ハイドロキノンモノメチルエーテル)を0.19部仕込み、乾燥空気を吹き込み(20ml/min)ながら80℃に昇温し均一になるまで撹拌した。均一になったところでクラレ社製アクリル酸27.5部、触媒として塩化ベンジルトリフェニルホスホニウム(北興化学工業社製、商品名TPP−ZC)を1.24部加え110℃で温度調整しながら7時間反応させ、酸価が7.8mgKOH/gのところで終了し、オリゴマー(1)(トルエン溶液)を得た。
蒸留装置のついた容量2リットルの三つ口フラスコに、1,4−シクロヘキサンジカルボン酸ジアリル1625g、プロピレングリコール327g、ジブチル錫オキサイド0.813gを仕込み、窒素気流下、180℃で生成してくるアルコールを留去しながら加熱した。留去したアルコールが約350gになったところで反応系内を徐々に(約4時間かけて)、6.6kPaまで減圧し、アリルアルコールの留出速度を速めた。留出液が殆ど出なくなったところで、反応系内を0.5kPaに減圧し、さらに1時間反応させた後、反応物を室温へと冷却した。以下、これにより得られた反応物をオリゴマー(2)とする。
100mlサンプル瓶にトルエン24gを入れ、そこにトリオクチルメチルアンモニウム塩でカチオン交換処理された親油性合成スメクタイト(コープケミカル社製合成スメクタイトSTN:数平均粒子径50nm、アスペクト比50、無機成分71%)3gをスターラーで撹拌しつつ少量ずつ加えた。さらにサンプル瓶にふたをし、ミックスローターにて室温下、1日間撹拌し、スメクタイト分散液を得た。このスメクタイト分散液にオリゴマー(1)のトルエン溶液(樹脂量換算7g)を加え、さらにUV硬化剤(チバ・スペシャルティ・ケミカルズ社製IRGACURE651)を0.35g加え十分撹拌し組成物(1)とした。組成物(1)をエバポレーターに取り付け、室温下20kPaにて10分間撹拌し、粘度調整及び組成物中のガス成分を除去した。
オリゴマー(1)をビスフェノールA型ビニルエステル樹脂(昭和高分子社製、商品名SP−1529X)に変えた以外は、実施例1と同様の操作を行った。しかし、ビニルエステル樹脂を加えると、合成スメクタイト分散液中で凝集してしまった。この分散液をPET上に塗布・乾燥を行ったが、均一に塗布することが出来ず、フィルムサンプルを得ることができなかった。
オリゴマー(1)をオリゴマー(2)(樹脂量7g)に変え、UV照射量を3000J/cm2に変更した以外は、実施例1と同様の操作を行い、サンプルフィルム(3)を得た。このフィルムの線膨張係数は84ppm/℃であり、Tgは検出されなかった。また、全光線透過率は91%であり、ヘーズは2.1%であった。
前記親油性合成スメクタイトを、ジメチルジオクタデシルアンモニウム塩でカチオン交換処理された親油性天然スメクタイト(ホージュン社製天然スメクタイトエスベンNX:無機成分58%)に変えた以外は、実施例1と同様の操作を行い、サンプルフィルム(4)を得た。このフィルムの線膨張係数は141ppm/℃であり、Tgは検出されなかった。また、全光線透過率は88%であり、ヘーズは21.3%であった。
Claims (13)
- 脂肪族エポキシ化合物から合成されるビニルエステル樹脂を含むビニルエステル樹脂組成物60質量%〜90質量%に、4級アンモニウム塩及び/または4級ホスホニウム塩によって有機化処理された数平均粒径が10nm〜300nmであり、アスペクト比が10〜300である合成スメクタイト10質量%〜40質量%を分散させた組成物を硬化してなることを特徴とする透明複合材料。
- 前記ビニルエステル樹脂が、脂環式構造を有するエポキシ化合物から合成されるビニルエステル樹脂である請求項1に記載の透明複合材料。
- 前記ビニルエステル樹脂が、水素化ビスフェノールA型エポキシ樹脂から合成されるビニルエステル樹脂である請求項1または2に記載の透明複合材料。
- 前記ビニルエステル樹脂組成物が、ビニルエステル樹脂30質量%〜100質量%とエチレン性不飽和基を有する反応性モノマー0質量%〜70質量%とから構成される請求項1に記載の透明複合材料。
- 前記合成スメクタイトが、合成ヘクトライト、合成サポナイト、及び合成スティーブンサイトから選択される1種以上である請求項1に記載の透明複合材料。
- 前記合成スメクタイトを有機化処理するための4級アンモニウム塩が、ラウリルトリメチルアンモニウム塩、ステアリルトリメチルアンモニウム塩、トリオクチルメチルアンモニウム塩、ジステアリルジメチルアンモニウム塩、ジ硬化牛脂ジメチルアンモニウム塩、ジステアリルジベンジルアンモニウム塩、及びN−ポリオキシエチレン−N−ラウリル−N,N−ジメチルアンモニウム塩の1種以上から選択される請求項1に記載の透明複合材料。
- 合成スメクタイトの表面に存在する水酸基が、表面改質剤によって処理されたものである請求項1、5または6に記載の透明複合材料。
- 前記表面改質剤が、シランカップリング剤、チタネートカップリング剤、グリシジル化合物、イソシアネート化合物、カルボン酸類、及びアルコール類から選択されるものである請求項7に記載の透明複合材料。
- 50℃〜250℃での面方向の平均線膨張係数が30ppm/℃以下で、かつ100μm厚当たりでの全光線透過率が85%以上である請求項1に記載の透明複合材料からなる透明板。
- 硬化前のビニルエステル樹脂組成物、合成スメクタイト、及び溶剤を含む組成物を、表面が平滑な平面上に塗布した後、溶剤を乾燥し、表面が平滑なシートまたはフィルムで挟み、電子線(EB)、紫外線(UV)または熱硬化させる請求項1に記載の透明複合材料の製造方法。
- 請求項1〜8のいずれかに記載の透明複合材料を基材とした表示装置。
- 前記表示装置が、液晶ディスプレイ、有機ELディスプレイ、または電子ペーパーである請求項11に記載の表示装置。
- 請求項1〜8のいずれかに記載の透明複合材料を基材とした太陽電池用基板。
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US9416294B2 (en) * | 2012-04-30 | 2016-08-16 | H.B. Fuller Company | Curable epoxide containing formaldehyde-free compositions, articles including the same, and methods of using the same |
CN102816461B (zh) * | 2012-08-27 | 2014-10-29 | 暨南大学 | 含季铵阳离子和季鏻阳离子的改性粘土及其制备与应用 |
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