JP6599726B2 - Polycarbonate resin composition and optical member - Google Patents
Polycarbonate resin composition and optical member Download PDFInfo
- Publication number
- JP6599726B2 JP6599726B2 JP2015209019A JP2015209019A JP6599726B2 JP 6599726 B2 JP6599726 B2 JP 6599726B2 JP 2015209019 A JP2015209019 A JP 2015209019A JP 2015209019 A JP2015209019 A JP 2015209019A JP 6599726 B2 JP6599726 B2 JP 6599726B2
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- Prior art keywords
- polycarbonate resin
- resin composition
- optical
- present
- refractive index
- Prior art date
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- 229920005668 polycarbonate resin Polymers 0.000 title claims description 119
- 239000004431 polycarbonate resin Substances 0.000 title claims description 119
- 239000000203 mixture Substances 0.000 title claims description 69
- 230000003287 optical effect Effects 0.000 title claims description 45
- 238000005452 bending Methods 0.000 claims description 21
- 239000010408 film Substances 0.000 description 28
- 238000000034 method Methods 0.000 description 26
- 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 14
- 238000000465 moulding Methods 0.000 description 14
- 239000008188 pellet Substances 0.000 description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- -1 spiroglycol Chemical compound 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 9
- 150000002009 diols Chemical class 0.000 description 8
- 238000004898 kneading Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000001746 injection moulding Methods 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229910052796 boron Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- ROORDVPLFPIABK-UHFFFAOYSA-N diphenyl carbonate Chemical compound C=1C=CC=CC=1OC(=O)OC1=CC=CC=C1 ROORDVPLFPIABK-UHFFFAOYSA-N 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 4
- 230000004075 alteration Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 150000004650 carbonic acid diesters Chemical class 0.000 description 4
- 238000000748 compression moulding Methods 0.000 description 4
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000002685 polymerization catalyst Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical class C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 3
- 229930185605 Bisphenol Natural products 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 150000001339 alkali metal compounds Chemical class 0.000 description 3
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000012788 optical film Substances 0.000 description 3
- 229920000515 polycarbonate Polymers 0.000 description 3
- 239000004417 polycarbonate Substances 0.000 description 3
- 239000011342 resin composition Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000007493 shaping process Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005809 transesterification reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PPTXVXKCQZKFBN-UHFFFAOYSA-N (S)-(-)-1,1'-Bi-2-naphthol Chemical compound C1=CC=C2C(C3=C4C=CC=CC4=CC=C3O)=C(O)C=CC2=C1 PPTXVXKCQZKFBN-UHFFFAOYSA-N 0.000 description 2
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- ZDSPTFQHKJLGFQ-UHFFFAOYSA-N 10,10-bis(4-hydroxyphenyl)anthracen-9-one Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)C2=CC=CC=C21 ZDSPTFQHKJLGFQ-UHFFFAOYSA-N 0.000 description 2
- RVSHVBMXBWNNPQ-UHFFFAOYSA-N 2-[1-(2-hydroxyethoxy)naphthalen-2-yl]oxyethanol Chemical compound C1=CC=CC2=C(OCCO)C(OCCO)=CC=C21 RVSHVBMXBWNNPQ-UHFFFAOYSA-N 0.000 description 2
- UTNSTOOXQPHXJQ-UHFFFAOYSA-N 2-[4-[4-(2-hydroxyethoxy)phenyl]sulfonylphenoxy]ethanol Chemical compound C1=CC(OCCO)=CC=C1S(=O)(=O)C1=CC=C(OCCO)C=C1 UTNSTOOXQPHXJQ-UHFFFAOYSA-N 0.000 description 2
- NQXNYVAALXGLQT-UHFFFAOYSA-N 2-[4-[9-[4-(2-hydroxyethoxy)phenyl]fluoren-9-yl]phenoxy]ethanol Chemical compound C1=CC(OCCO)=CC=C1C1(C=2C=CC(OCCO)=CC=2)C2=CC=CC=C2C2=CC=CC=C21 NQXNYVAALXGLQT-UHFFFAOYSA-N 0.000 description 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 2
- BQPBZDSDFCDSAO-UHFFFAOYSA-N 2-naphthalen-2-yloxyethanol Chemical compound C1=CC=CC2=CC(OCCO)=CC=C21 BQPBZDSDFCDSAO-UHFFFAOYSA-N 0.000 description 2
- YMTYZTXUZLQUSF-UHFFFAOYSA-N 3,3'-Dimethylbisphenol A Chemical compound C1=C(O)C(C)=CC(C(C)(C)C=2C=C(C)C(O)=CC=2)=C1 YMTYZTXUZLQUSF-UHFFFAOYSA-N 0.000 description 2
- VWGKEVWFBOUAND-UHFFFAOYSA-N 4,4'-thiodiphenol Chemical compound C1=CC(O)=CC=C1SC1=CC=C(O)C=C1 VWGKEVWFBOUAND-UHFFFAOYSA-N 0.000 description 2
- UMPGNGRIGSEMTC-UHFFFAOYSA-N 4-[1-(4-hydroxyphenyl)-3,3,5-trimethylcyclohexyl]phenol Chemical compound C1C(C)CC(C)(C)CC1(C=1C=CC(O)=CC=1)C1=CC=C(O)C=C1 UMPGNGRIGSEMTC-UHFFFAOYSA-N 0.000 description 2
- PVFQHGDIOXNKIC-UHFFFAOYSA-N 4-[2-[3-[2-(4-hydroxyphenyl)propan-2-yl]phenyl]propan-2-yl]phenol Chemical compound C=1C=CC(C(C)(C)C=2C=CC(O)=CC=2)=CC=1C(C)(C)C1=CC=C(O)C=C1 PVFQHGDIOXNKIC-UHFFFAOYSA-N 0.000 description 2
- NUDSREQIJYWLRA-UHFFFAOYSA-N 4-[9-(4-hydroxy-3-methylphenyl)fluoren-9-yl]-2-methylphenol Chemical compound C1=C(O)C(C)=CC(C2(C3=CC=CC=C3C3=CC=CC=C32)C=2C=C(C)C(O)=CC=2)=C1 NUDSREQIJYWLRA-UHFFFAOYSA-N 0.000 description 2
- 125000004203 4-hydroxyphenyl group Chemical group [H]OC1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VOWWYDCFAISREI-UHFFFAOYSA-N Bisphenol AP Chemical compound C=1C=C(O)C=CC=1C(C=1C=CC(O)=CC=1)(C)C1=CC=CC=C1 VOWWYDCFAISREI-UHFFFAOYSA-N 0.000 description 2
- SDDLEVPIDBLVHC-UHFFFAOYSA-N Bisphenol Z Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)CCCCC1 SDDLEVPIDBLVHC-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- KLDXJTOLSGUMSJ-JGWLITMVSA-N Isosorbide Chemical compound O[C@@H]1CO[C@@H]2[C@@H](O)CO[C@@H]21 KLDXJTOLSGUMSJ-JGWLITMVSA-N 0.000 description 2
- JMMSLMMJRMCXPW-UHFFFAOYSA-N OC.OC.C1CC2CCC1C2 Chemical compound OC.OC.C1CC2CCC1C2 JMMSLMMJRMCXPW-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- AYVGBNGTBQLJBG-UHFFFAOYSA-N [3-(hydroxymethyl)cyclopentyl]methanol Chemical compound OCC1CCC(CO)C1 AYVGBNGTBQLJBG-UHFFFAOYSA-N 0.000 description 2
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 2
- KBWLBXSZWRTHKM-UHFFFAOYSA-N [6-(hydroxymethyl)-1,2,3,4,4a,5,6,7,8,8a-decahydronaphthalen-2-yl]methanol Chemical compound C1C(CO)CCC2CC(CO)CCC21 KBWLBXSZWRTHKM-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 125000006267 biphenyl group Chemical group 0.000 description 2
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical class [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- MHIBEGOZTWERHF-UHFFFAOYSA-N heptane-1,1-diol Chemical compound CCCCCCC(O)O MHIBEGOZTWERHF-UHFFFAOYSA-N 0.000 description 2
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 229960002479 isosorbide Drugs 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- NXPPAOGUKPJVDI-UHFFFAOYSA-N naphthalene-1,2-diol Chemical compound C1=CC=CC2=C(O)C(O)=CC=C21 NXPPAOGUKPJVDI-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- FVXBCDWMKCEPCL-UHFFFAOYSA-N nonane-1,1-diol Chemical compound CCCCCCCCC(O)O FVXBCDWMKCEPCL-UHFFFAOYSA-N 0.000 description 2
- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 150000004714 phosphonium salts Chemical group 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical compound CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 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
- VLCQYXZALXDPEV-UHFFFAOYSA-N (2,3,4-triethylphenyl)boron Chemical compound [B]C1=CC=C(CC)C(CC)=C1CC VLCQYXZALXDPEV-UHFFFAOYSA-N 0.000 description 1
- PJAWEFMLSSLAIM-UHFFFAOYSA-N (2,3,4-trimethylphenyl)boron Chemical compound [B]C1=CC=C(C)C(C)=C1C PJAWEFMLSSLAIM-UHFFFAOYSA-N 0.000 description 1
- IHPFDBSMYWRYHQ-UHFFFAOYSA-N (2-benzylphenyl)-diphenylborane Chemical compound C=1C=CC=C(B(C=2C=CC=CC=2)C=2C=CC=CC=2)C=1CC1=CC=CC=C1 IHPFDBSMYWRYHQ-UHFFFAOYSA-N 0.000 description 1
- GCLVVFYKIZYIIL-UHFFFAOYSA-N (2-butylphenyl)-diphenylborane Chemical compound CCCCC1=CC=CC=C1B(C=1C=CC=CC=1)C1=CC=CC=C1 GCLVVFYKIZYIIL-UHFFFAOYSA-N 0.000 description 1
- KBIWOGUYLGWUTF-UHFFFAOYSA-N (2-methylphenyl)-diphenylborane Chemical compound CC1=CC=CC=C1B(C=1C=CC=CC=1)C1=CC=CC=C1 KBIWOGUYLGWUTF-UHFFFAOYSA-N 0.000 description 1
- GPFJHNSSBHPYJK-UHFFFAOYSA-N (3-methylphenyl) hydrogen carbonate Chemical compound CC1=CC=CC(OC(O)=O)=C1 GPFJHNSSBHPYJK-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- XGVZPMZEBYEFAD-UHFFFAOYSA-N 2,2-dimethylpropylboron Chemical compound [B]CC(C)(C)C XGVZPMZEBYEFAD-UHFFFAOYSA-N 0.000 description 1
- QUMMIJOYXPIWKT-UHFFFAOYSA-N 2-(2-methylphenyl)propan-2-ylboron Chemical compound [B]C(C)(C)C1=CC=CC=C1C QUMMIJOYXPIWKT-UHFFFAOYSA-N 0.000 description 1
- HBTONAMIPDVQRI-UHFFFAOYSA-N 2-[4-[9-[4-(2-hydroxyethoxy)-3-phenylphenyl]fluoren-9-yl]-2-phenylphenoxy]ethanol Chemical compound OCCOC1=CC=C(C2(C3=CC=CC=C3C3=CC=CC=C32)C=2C=C(C(OCCO)=CC=2)C=2C=CC=CC=2)C=C1C1=CC=CC=C1 HBTONAMIPDVQRI-UHFFFAOYSA-N 0.000 description 1
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 description 1
- NJMIRMHNYQIHST-UHFFFAOYSA-M 2-dodecylbenzenesulfonate;tetrabutylphosphanium Chemical compound CCCC[P+](CCCC)(CCCC)CCCC.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O NJMIRMHNYQIHST-UHFFFAOYSA-M 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 2-phenyl-1h-imidazole Chemical compound C1=CNC(C=2C=CC=CC=2)=N1 ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 0.000 description 1
- CCZFANLSRKSNMX-UHFFFAOYSA-N 3-(2-ethylphenyl)pentan-3-ylboron Chemical compound CCC([B])(CC)C1=CC=CC=C1CC CCZFANLSRKSNMX-UHFFFAOYSA-N 0.000 description 1
- PQXOTHUSZUHPBK-UHFFFAOYSA-N 3-ethylpentan-3-ylboron Chemical compound CCC([B])(CC)CC PQXOTHUSZUHPBK-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- HXFVOUUOTHJFPX-UHFFFAOYSA-N alumane;zinc Chemical class [AlH3].[Zn] HXFVOUUOTHJFPX-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 150000001463 antimony compounds Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- UCVMQZHZWWEPRC-UHFFFAOYSA-L barium(2+);hydrogen carbonate Chemical compound [Ba+2].OC([O-])=O.OC([O-])=O UCVMQZHZWWEPRC-UHFFFAOYSA-L 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 description 1
- MUCRFDZUHPMASM-UHFFFAOYSA-N bis(2-chlorophenyl) carbonate Chemical compound ClC1=CC=CC=C1OC(=O)OC1=CC=CC=C1Cl MUCRFDZUHPMASM-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- FLLNLJJKHKZKMB-UHFFFAOYSA-N boron;tetramethylazanium Chemical compound [B].C[N+](C)(C)C FLLNLJJKHKZKMB-UHFFFAOYSA-N 0.000 description 1
- QYJXDIUNDMRLAO-UHFFFAOYSA-N butyl 4-methylbenzenesulfonate Chemical compound CCCCOS(=O)(=O)C1=CC=C(C)C=C1 QYJXDIUNDMRLAO-UHFFFAOYSA-N 0.000 description 1
- NIKBCKTWWPVAIC-UHFFFAOYSA-N butyl benzenesulfonate Chemical compound CCCCOS(=O)(=O)C1=CC=CC=C1 NIKBCKTWWPVAIC-UHFFFAOYSA-N 0.000 description 1
- ZOAIGCHJWKDIPJ-UHFFFAOYSA-M caesium acetate Chemical compound [Cs+].CC([O-])=O ZOAIGCHJWKDIPJ-UHFFFAOYSA-M 0.000 description 1
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 1
- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- BLUMOBPWAAOPOY-UHFFFAOYSA-M cesium;benzoate Chemical compound [Cs+].[O-]C(=O)C1=CC=CC=C1 BLUMOBPWAAOPOY-UHFFFAOYSA-M 0.000 description 1
- WLZGEDNSZCPRCJ-UHFFFAOYSA-M cesium;octadecanoate Chemical compound [Cs+].CCCCCCCCCCCCCCCCCC([O-])=O WLZGEDNSZCPRCJ-UHFFFAOYSA-M 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- SMBQBQBNOXIFSF-UHFFFAOYSA-N dilithium Chemical compound [Li][Li] SMBQBQBNOXIFSF-UHFFFAOYSA-N 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- TYJOJLOWRIQYQM-UHFFFAOYSA-L disodium;phenyl phosphate Chemical compound [Na+].[Na+].[O-]P([O-])(=O)OC1=CC=CC=C1 TYJOJLOWRIQYQM-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000007688 edging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XDRMBCMMABGNMM-UHFFFAOYSA-N ethyl benzenesulfonate Chemical compound CCOS(=O)(=O)C1=CC=CC=C1 XDRMBCMMABGNMM-UHFFFAOYSA-N 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 150000002291 germanium compounds Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 229940031993 lithium benzoate Drugs 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 description 1
- LDJNSLOKTFFLSL-UHFFFAOYSA-M lithium;benzoate Chemical compound [Li+].[O-]C(=O)C1=CC=CC=C1 LDJNSLOKTFFLSL-UHFFFAOYSA-M 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 description 1
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 description 1
- 239000002370 magnesium bicarbonate Substances 0.000 description 1
- 235000014824 magnesium bicarbonate Nutrition 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 150000002697 manganese compounds Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000005499 meniscus Effects 0.000 description 1
- 239000006078 metal deactivator Substances 0.000 description 1
- VUQUOGPMUUJORT-UHFFFAOYSA-N methyl 4-methylbenzenesulfonate Chemical compound COS(=O)(=O)C1=CC=C(C)C=C1 VUQUOGPMUUJORT-UHFFFAOYSA-N 0.000 description 1
- CZXGXYBOQYQXQD-UHFFFAOYSA-N methyl benzenesulfonate Chemical compound COS(=O)(=O)C1=CC=CC=C1 CZXGXYBOQYQXQD-UHFFFAOYSA-N 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- KDQQMEAEIKFPLQ-UHFFFAOYSA-N n-(1-cyanocyclohexyl)-2-fluorobenzamide Chemical compound FC1=CC=CC=C1C(=O)NC1(C#N)CCCCC1 KDQQMEAEIKFPLQ-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- GVMDZMPQYYHMSV-UHFFFAOYSA-N octyl benzenesulfonate Chemical compound CCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVMDZMPQYYHMSV-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- RKHQZMOCQHXUBC-UHFFFAOYSA-N phenol;potassium Chemical compound [K].OC1=CC=CC=C1 RKHQZMOCQHXUBC-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- KZQFPRKQBWRRHQ-UHFFFAOYSA-N phenyl 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)OC1=CC=CC=C1 KZQFPRKQBWRRHQ-UHFFFAOYSA-N 0.000 description 1
- CGEXUOTXYSGBLV-UHFFFAOYSA-N phenyl benzenesulfonate Chemical compound C=1C=CC=CC=1S(=O)(=O)OC1=CC=CC=C1 CGEXUOTXYSGBLV-UHFFFAOYSA-N 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 235000010235 potassium benzoate Nutrition 0.000 description 1
- 239000004300 potassium benzoate Substances 0.000 description 1
- 229940103091 potassium benzoate Drugs 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 229940114930 potassium stearate Drugs 0.000 description 1
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 description 1
- 229910001866 strontium hydroxide Inorganic materials 0.000 description 1
- 159000000008 strontium salts Chemical class 0.000 description 1
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- BJQWBACJIAKDTJ-UHFFFAOYSA-N tetrabutylphosphanium Chemical class CCCC[P+](CCCC)(CCCC)CCCC BJQWBACJIAKDTJ-UHFFFAOYSA-N 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 description 1
- IGNTWNVBGLNYDV-UHFFFAOYSA-N triisopropylphosphine Chemical compound CC(C)P(C(C)C)C(C)C IGNTWNVBGLNYDV-UHFFFAOYSA-N 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
- KCTAHLRCZMOTKM-UHFFFAOYSA-N tripropylphosphane Chemical compound CCCP(CCC)CCC KCTAHLRCZMOTKM-UHFFFAOYSA-N 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
本発明は、高屈折率、低複屈折であり、かつ、表面硬度と耐折り曲げ性のバランスに優れたポリカーボネート樹脂組成物に関する。また、該ポリカーボネート樹脂組成物からなる光学部材に関する。 The present invention relates to a polycarbonate resin composition having a high refractive index and low birefringence, and having an excellent balance between surface hardness and bending resistance. Moreover, it is related with the optical member which consists of this polycarbonate resin composition.
2,2−ビス(4−ヒドロキシフェニル)プロパン(通称ビスフェノールA)とホスゲンあるいは炭酸ジフェニルなどの炭酸エステル形成性化合物と反応させて製造される従来のポリカーボネート樹脂は、透明性が高く、耐熱性や耐衝撃性に優れるため、光ディスク等の光学部材に使用されてきた。しかしながら、複屈折が大きいことや表面が傷つきやすいといった欠点があり、使用用途が限られていた。複屈折を小さくする方法として、側鎖にフルオレン構造を有するビスフェノール類の共重合が報告されている。(特許文献1,2,3)。しかしながら、特許文献1のポリカーボネート樹脂は、溶融時の粘度が極めて高く、光学レンズや光ディスクなどを成形するのは困難である。また、特許文献2や特許文献3のポリカーボネート樹脂は、成形上の問題のない溶融粘度を有するポリカーボネートであり、光ディスクに好適との記載があるが、光学レンズに使用するには屈折率が不十分であった。また、表面硬度が低く傷つきやすいため、使用用途によっては問題があった。
A conventional polycarbonate resin produced by reacting 2,2-bis (4-hydroxyphenyl) propane (commonly called bisphenol A) with a carbonate ester-forming compound such as phosgene or diphenyl carbonate has high transparency, heat resistance, Since it has excellent impact resistance, it has been used for optical members such as optical disks. However, there are drawbacks such as large birefringence and the surface being easily damaged, and the usage is limited. As a method for reducing birefringence, the copolymerization of bisphenols having a fluorene structure in the side chain has been reported. (
そこで、さらに高屈折率であるポリカーボネート樹脂が提案されている(特許文献4,5)。しかしながら、特許文献4,5に記載のポリカーボネート樹脂は脆いため、射出成形時に成形片やスプルーが折れやすいという問題があった。また、光学フィルムとして使用する際に、耐折り曲げ性が不十分であるといった問題もあった。 Therefore, a polycarbonate resin having a higher refractive index has been proposed (Patent Documents 4 and 5). However, since the polycarbonate resins described in Patent Documents 4 and 5 are brittle, there is a problem that the molded piece and the sprue are easily broken during injection molding. Moreover, when using as an optical film, there also existed a problem that bending resistance was inadequate.
そこで本発明の目的は、高屈折率、低複屈折であり、かつ、表面硬度と耐折り曲げ性のバランスに優れたポリカーボネート樹脂組成物を提供することにある。また、該ポリカーボネート樹脂組成物からなる光学部材を提供することにある。 Therefore, an object of the present invention is to provide a polycarbonate resin composition having a high refractive index and a low birefringence and having an excellent balance between surface hardness and bending resistance. Moreover, it is providing the optical member which consists of this polycarbonate resin composition.
本発明者らはこの目的を達成せんとして鋭意研究を重ねた結果、下記ポリカーボネート樹脂組成物及び光学部材によって、上記課題を解決することができることを見出し本発明に到達した。 The inventors of the present invention have intensively studied to achieve this object, and as a result, have found that the above problems can be solved by the following polycarbonate resin composition and optical member, and have reached the present invention.
すなわち、本発明は、
1.式(1)で表される構成単位を有するポリカーボネート樹脂(A)と式(2)で表される構成単位を有するポリカーボネート樹脂(B)を含むポリカーボネート樹脂組成物。
3.ポリカーボネート樹脂(A)とポリカーボネート樹脂(B)の重量比率(100×(A))/((A)+(B))が、20〜80wt%である上記1または2のいずれかに記載のポリカーボネート樹脂組成物。
4.比粘度が0.12〜0.40である上記1〜3のいずれかに記載のポリカーボネート樹脂組成物。
5.屈折率が1.640〜1.660である上記1〜4のいずれかに記載のポリカーボネート樹脂組成物。
6.配向複屈折の絶対値が6×10−3以下である上記1〜5のいずれかに記載のポリカーボネート樹脂組成物。
7.耐折り曲げ性が20mm以下である上記1〜6のいずれかに記載のポリカーボネート樹脂組成物。
8.鉛筆硬度がF以上である上記1〜7のいずれかに記載のポリカーボネート樹脂組成物。
9.前記1〜8のいずれかに記載のポリカーボネート樹脂組成物からなる光学部材。
10.前記1〜8のいずれかに記載のポリカーボネート樹脂組成物からなる光学レンズ。
11.前記1〜8のいずれかに記載のポリカーボネート樹脂組成物からなる透明フィルム。
That is, the present invention
1. A polycarbonate resin composition comprising a polycarbonate resin (A) having a structural unit represented by formula (1) and a polycarbonate resin (B) having a structural unit represented by formula (2).
3. 3. The polycarbonate according to any one of 1 or 2 above, wherein the weight ratio (100 × (A)) / ((A) + (B)) of the polycarbonate resin (A) to the polycarbonate resin (B) is 20 to 80 wt%. Resin composition.
4). 4. The polycarbonate resin composition according to any one of the above 1 to 3, having a specific viscosity of 0.12 to 0.40.
5. The polycarbonate resin composition according to any one of the above 1 to 4, wherein the refractive index is 1.640 to 1.660.
6). The polycarbonate resin composition according to any one of 1 to 5 above, wherein the absolute value of orientation birefringence is 6 × 10 −3 or less.
7). The polycarbonate resin composition according to any one of 1 to 6 above, wherein the bending resistance is 20 mm or less.
8). The polycarbonate resin composition according to any one of 1 to 7 above, wherein the pencil hardness is F or more.
9. The optical member which consists of a polycarbonate resin composition in any one of said 1-8.
10. The optical lens which consists of a polycarbonate resin composition in any one of said 1-8.
11. The transparent film which consists of a polycarbonate resin composition in any one of said 1-8.
本発明のポリカーボネート樹脂組成物及び光学部材は、高屈折率、低複屈折であり、かつ、表面硬度と耐折り曲げ性のバランスに優れるため、その奏する産業上の効果は、格別である。 Since the polycarbonate resin composition and the optical member of the present invention have a high refractive index and a low birefringence and are excellent in the balance between the surface hardness and the bending resistance, the industrial effect exerted by them is exceptional.
以下、本発明の実施形態について具体的に説明する。
〈ポリカーボネート樹脂組成物〉
本発明のポリカーボネート樹脂組成物は、式(1)で表される構成単位を含むポリカーボネート樹脂(A)と式(2)で表される構成単位を含むポリカーボネート樹脂(B)を含む。
本発明のポリカーボネート樹脂組成物におけるポリカーボネート樹脂(A)とポリカーボネート樹脂(B)の重量比率(100×(A))/((A)+(B))は、10〜90wt%であることが好ましく、20〜80wt%であるとより好ましく、30〜70wt%であるとよりいっそう好ましく、50〜70wt%であるとさらに好ましい。重量比率が上記範囲内であると、高屈折率、低複屈折であり、表面硬度と耐折り曲げ性のバランスに優れるため好ましい。
Hereinafter, embodiments of the present invention will be specifically described.
<Polycarbonate resin composition>
The polycarbonate resin composition of the present invention includes a polycarbonate resin (A) containing a structural unit represented by the formula (1) and a polycarbonate resin (B) containing a structural unit represented by the formula (2).
The weight ratio (100 × (A)) / ((A) + (B)) of the polycarbonate resin (A) and the polycarbonate resin (B) in the polycarbonate resin composition of the present invention is preferably 10 to 90 wt%. More preferably, it is 20-80 wt%, More preferably, it is 30-70 wt%, More preferably, it is 50-70 wt%. It is preferable for the weight ratio to be in the above-mentioned range since it has a high refractive index and low birefringence and is excellent in the balance between surface hardness and bending resistance.
本発明のポリカーボネート樹脂組成物に使用するポリカーボネート樹脂(A)は、式(1)で表される構成単位を主に含むが、本発明の特性を損なわい程度に他のジオール成分を共重合してもよい。他のジオール成分は、全繰り返し単位中10mol%以下が好ましい。その他のジオール成分として、エチレングリコール、プロパンジオール、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、オクタンジオール、ノナンジオール、トリシクロ[5.2.1.02,6]デカンジメタノール、シクロヘキサン−1,4−ジメタノール、デカリン−2,6−ジメタノール、ノルボルナンジメタノール、ペンタシクロペンタデカンジメタノール、シクロペンタン−1,3−ジメタノール、スピログリコール、イソソルビド、ヒドロキノン、レゾルシノール、2,2−ビス(4−ヒドロキシフェニル)プロパン、2,2−ビス(3−メチル−4−ヒドロキシフェニル)プロパン、1,1−ビス(4−ヒドロキシフェニル)−1−フェニルエタン、ビス(4−ヒドロキシフェニル)ジフェニルメタン、1,3−ビス(2−(4−ヒドロキシフェニル)−2−プロピル)ベンゼン、ビス(4−ヒドロキシフェニル)スルホン、ビス(4−(2−ヒドロキシエトキシ)フェニル)スルホン、ビス(4−ヒドロキシフェニル)スルフィド、1,1−ビス(4−ヒドロキシフェニル)−3,3,5−トリメチルシクロヘキサン、1,1−ビス(4−ヒドロキシフェニル)シクロヘキサン、ビフェノール、ビスフェノールフルオレン、ビスクレゾールフルオレン、1,1−ビ(2−(2−ヒドロキシエトキシ)ナフタレン)、1,1−ビ−2−ナフトール、ジヒドロキシナフタレン、ビス(2−ヒドロキシエトキシ)ナフタレン、10,10−ビス(4−ヒドロキシフェニル)アントロン等が挙げられる。 The polycarbonate resin (A) used in the polycarbonate resin composition of the present invention mainly contains the structural unit represented by the formula (1), but is copolymerized with other diol components to such an extent that the characteristics of the present invention are not impaired. May be. The other diol component is preferably 10 mol% or less in all repeating units. Other diol components include ethylene glycol, propanediol, butanediol, pentanediol, hexanediol, heptanediol, octanediol, nonanediol, tricyclo [5.2.1.02,6] decandimethanol, cyclohexane-1, 4-dimethanol, decalin-2,6-dimethanol, norbornane dimethanol, pentacyclopentadecanedimethanol, cyclopentane-1,3-dimethanol, spiroglycol, isosorbide, hydroquinone, resorcinol, 2,2-bis (4 -Hydroxyphenyl) propane, 2,2-bis (3-methyl-4-hydroxyphenyl) propane, 1,1-bis (4-hydroxyphenyl) -1-phenylethane, bis (4-hydroxyphenyl) diphenyl Tan, 1,3-bis (2- (4-hydroxyphenyl) -2-propyl) benzene, bis (4-hydroxyphenyl) sulfone, bis (4- (2-hydroxyethoxy) phenyl) sulfone, bis (4- Hydroxyphenyl) sulfide, 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane, 1,1-bis (4-hydroxyphenyl) cyclohexane, biphenol, bisphenol fluorene, biscresol fluorene, 1, 1-bi (2- (2-hydroxyethoxy) naphthalene), 1,1-bi-2-naphthol, dihydroxynaphthalene, bis (2-hydroxyethoxy) naphthalene, 10,10-bis (4-hydroxyphenyl) anthrone, etc. Is mentioned.
本発明のポリカーボネート樹脂組成物に使用するポリカーボネート樹脂(B)は、式(2)で表される構成単位を主に含むが、本発明の特性を損なわい程度に他のジオール成分を共重合してもよい。他のジオール成分は、全繰り返し単位中10mol%以下が好ましい。その他のジオール成分として、エチレングリコール、プロパンジオール、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、オクタンジオール、ノナンジオール、トリシクロ[5.2.1.02,6]デカンジメタノール、シクロヘキサン−1,4−ジメタノール、デカリン−2,6−ジメタノール、ノルボルナンジメタノール、ペンタシクロペンタデカンジメタノール、シクロペンタン−1,3−ジメタノール、スピログリコール、イソソルビド、ヒドロキノン、レゾルシノール、2,2−ビス(4−ヒドロキシフェニル)プロパン、2,2−ビス(3−メチル−4−ヒドロキシフェニル)プロパン、1,1−ビス(4−ヒドロキシフェニル)−1−フェニルエタン、ビス(4−ヒドロキシフェニル)ジフェニルメタン、1,3−ビス(2−(4−ヒドロキシフェニル)−2−プロピル)ベンゼン、ビス(4−ヒドロキシフェニル)スルホン、ビス(4−(2−ヒドロキシエトキシ)フェニル)スルホン、ビス(4−ヒドロキシフェニル)スルフィド、1,1−ビス(4−ヒドロキシフェニル)−3,3,5−トリメチルシクロヘキサン、1,1−ビス(4−ヒドロキシフェニル)シクロヘキサン、ビフェノール、ビスフェノールフルオレン、ビスクレゾールフルオレン、1,1−ビ(2−(2−ヒドロキシエトキシ)ナフタレン)、1,1−ビ−2−ナフトール、ジヒドロキシナフタレン、ビス(2−ヒドロキシエトキシ)ナフタレン、10,10−ビス(4−ヒドロキシフェニル)アントロン等が挙げられる。 The polycarbonate resin (B) used in the polycarbonate resin composition of the present invention mainly contains the structural unit represented by the formula (2), but is copolymerized with other diol components to such an extent that the characteristics of the present invention are not impaired. May be. The other diol component is preferably 10 mol% or less in all repeating units. Other diol components include ethylene glycol, propanediol, butanediol, pentanediol, hexanediol, heptanediol, octanediol, nonanediol, tricyclo [5.2.1.02,6] decandimethanol, cyclohexane-1, 4-dimethanol, decalin-2,6-dimethanol, norbornane dimethanol, pentacyclopentadecanedimethanol, cyclopentane-1,3-dimethanol, spiroglycol, isosorbide, hydroquinone, resorcinol, 2,2-bis (4 -Hydroxyphenyl) propane, 2,2-bis (3-methyl-4-hydroxyphenyl) propane, 1,1-bis (4-hydroxyphenyl) -1-phenylethane, bis (4-hydroxyphenyl) diphenyl Tan, 1,3-bis (2- (4-hydroxyphenyl) -2-propyl) benzene, bis (4-hydroxyphenyl) sulfone, bis (4- (2-hydroxyethoxy) phenyl) sulfone, bis (4- Hydroxyphenyl) sulfide, 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane, 1,1-bis (4-hydroxyphenyl) cyclohexane, biphenol, bisphenol fluorene, biscresol fluorene, 1, 1-bi (2- (2-hydroxyethoxy) naphthalene), 1,1-bi-2-naphthol, dihydroxynaphthalene, bis (2-hydroxyethoxy) naphthalene, 10,10-bis (4-hydroxyphenyl) anthrone, etc. Is mentioned.
本発明のポリカーボネート樹脂組成物の比粘度は、0.12〜0.40が好ましく、0.15〜0.35であるとさらに好ましく、0.18〜0.30であるとよりいっそう好ましい。比粘度が上記範囲内であると成形性と機械強度のバランスに優れるため好ましい。
本発明のポリカーボネート樹脂組成物の屈折率は、1.640〜1.660であると好ましく、1.641〜1.660であるとさらに好ましく、1.643〜1.660であるとよりいっそう好ましい。屈折率は25℃、波長589nmにおいて測定する。屈折率が1.635以上の場合、レンズの球面収差を低減でき、さらにレンズの焦点距離を短くする事ができるため好ましい。
The specific viscosity of the polycarbonate resin composition of the present invention is preferably 0.12 to 0.40, more preferably 0.15 to 0.35, and even more preferably 0.18 to 0.30. It is preferable for the specific viscosity to be in the above range since the balance between moldability and mechanical strength is excellent.
The refractive index of the polycarbonate resin composition of the present invention is preferably 1.640 to 1.660, more preferably 1.641 to 1.660, and even more preferably 1.643 to 1.660. . The refractive index is measured at 25 ° C. and wavelength 589 nm. A refractive index of 1.635 or more is preferable because the spherical aberration of the lens can be reduced and the focal length of the lens can be shortened.
本発明のポリカーボネート樹脂組成物のアッベ数(ν)は、19〜25であると好ましく、20〜24であるとさらに好ましい。アッベ数は25℃、波長486nm、589nm、656nmの屈折率から下記式を用いて算出する。
ν=(nD−1)/(nF−nC)
nD:波長589nmでの屈折率
nC:波長656nmでの屈折率
nF:波長486nmでの屈折率
The Abbe number (ν) of the polycarbonate resin composition of the present invention is preferably 19 to 25, and more preferably 20 to 24. The Abbe number is calculated from the refractive index at 25 ° C., wavelengths 486 nm, 589 nm, and 656 nm using the following formula.
v = (nD-1) / (nF-nC)
nD: Refractive index at a wavelength of 589 nm nC: Refractive index at a wavelength of 656 nm nF: Refractive index at a wavelength of 486 nm
本発明のポリカーボネート樹脂組成物は、配向複屈折(Δn)の絶対値が、好ましくは0〜6×10−3、より好ましくは0〜4×10−3、さらに好ましくは0〜2×10−3の範囲である。配向複屈折(Δn)は、該ポリカーボネート樹脂より得られる厚さ100μmのキャストフィルムをTg+10℃で2倍延伸した時、波長589nmにおいて測定する。配向複屈折が上記範囲内であると、レンズの光学歪が小さくなるため好ましい。 In the polycarbonate resin composition of the present invention, the absolute value of orientation birefringence (Δn) is preferably 0 to 6 × 10 −3 , more preferably 0 to 4 × 10 −3 , and still more preferably 0 to 2 × 10 −. 3 range. The orientation birefringence (Δn) is measured at a wavelength of 589 nm when a cast film having a thickness of 100 μm obtained from the polycarbonate resin is stretched twice at Tg + 10 ° C. It is preferable that the orientation birefringence is within the above range because the optical distortion of the lens becomes small.
本発明のポリカーボネート樹脂組成物は、1mm厚の全光線透過率が、好ましくは80%以上、より好ましくは85%以上、さらに好ましくは88%以上である。全光線透過率が上記範囲内であると、光学部材として適している。
本発明のポリカーボネート樹脂組成物は、23℃、24時間浸漬後の吸水率が0.25%以下であると好ましく、0.20%以下であるとより好ましい。吸水率が上記範囲内であると、吸水による光学特性の変化が小さいため好ましい。
The polycarbonate resin composition of the present invention has a total light transmittance of 1 mm thickness, preferably 80% or more, more preferably 85% or more, and still more preferably 88% or more. When the total light transmittance is within the above range, it is suitable as an optical member.
The polycarbonate resin composition of the present invention preferably has a water absorption rate of 0.25% or less after being immersed at 23 ° C. for 24 hours, more preferably 0.20% or less. It is preferable for the water absorption rate to be within the above range since the change in optical properties due to water absorption is small.
本発明のポリカーボネート樹脂組成物は、ガラス転移点(Tg)が120〜160℃であると好ましく、130〜160℃であるとより好ましい。ガラス転移点が上記範囲内であると、耐熱性と成形性のバランスに優れるため好ましい。
本発明のポリカーボネート樹脂組成物は、耐折り曲げ性が20mm以下であると好ましく、15mm以下であるとより好ましく、10mm以下であるとよりいっそう好ましい。
The polycarbonate resin composition of the present invention preferably has a glass transition point (Tg) of 120 to 160 ° C, more preferably 130 to 160 ° C. It is preferable for the glass transition point to be in the above-mentioned range because of excellent balance between heat resistance and moldability.
The polycarbonate resin composition of the present invention preferably has a bending resistance of 20 mm or less, more preferably 15 mm or less, and even more preferably 10 mm or less.
本発明のポリカーボネート樹脂の耐折り曲げ性とは、以下の方法により測定した値を示す。測定方法は、長さ40mm、幅10mm、厚さ100μmのフィルムを用いて、万力の左右の接合面の間隔を40mmに開き、前記試験片の両端を接合面内に固定した。次に左右の接合面の間隔を2mm/秒以下の速度で狭めていき、折れ曲がった試験片全体を該接合面内で圧縮した。そして、接合面間が完全に密着する迄に試験片が折れ曲がり部で2片(又は3片以上の破片)に割れた際、万力の接合面の移動を停止し、接合面の間隔を測定した。耐折り曲げ性の数値が大きいほど、フィルムが割れやすいことを示す。耐折り曲げ性が上記範囲内であると、光学部材として十分な機械強度があるため好ましい。 The bending resistance of the polycarbonate resin of the present invention is a value measured by the following method. The measuring method used the film of length 40mm, width 10mm, and thickness 100micrometer, opened the space | interval of the joint surface of a right and left vise to 40mm, and fixed the both ends of the said test piece in the joint surface. Next, the interval between the left and right joint surfaces was narrowed at a speed of 2 mm / second or less, and the entire bent test piece was compressed in the joint surface. And when the test piece is bent into two pieces (or more than three pieces) at the bent part until the joint surfaces are completely in close contact, the movement of the joint surface of the vise is stopped and the distance between the joint surfaces is measured. did. It shows that a film is easily broken, so that a numerical value of bending resistance is large. It is preferable for the bending resistance to be within the above range since there is sufficient mechanical strength as an optical member.
本発明のポリカーボネート樹脂組成物は、鉛筆硬度が好ましくはF以上、より好ましくはH以上である。鉛筆硬度とは、本発明のポリカーボネート樹脂を特定の鉛筆硬度を有する鉛筆で樹脂を擦過した場合に擦過しても擦過痕が残らない硬さのことであり、JIS K−5600に従って測定できる塗膜の表面硬度試験に用いる鉛筆硬度を指標とする。鉛筆硬度は、9H、8H、7H、6H、5H、4H、3H、2H、H、F、HB、B、2B、3B、4B、5B、6Bの順で柔らかくなり、最も硬いものが9H、最も軟らかいものが6Bである。 The polycarbonate resin composition of the present invention preferably has a pencil hardness of F or higher, more preferably H or higher. The pencil hardness is a hardness that does not leave a scratch mark even when the polycarbonate resin of the present invention is rubbed with a pencil having a specific pencil hardness, and can be measured according to JIS K-5600. The pencil hardness used for the surface hardness test is used as an index. Pencil hardness becomes soft in the order of 9H, 8H, 7H, 6H, 5H, 4H, 3H, 2H, H, F, HB, B, 2B, 3B, 4B, 5B, 6B, the hardest is 9H, The soft one is 6B.
〈ポリカーボネート樹脂の製造方法〉
本発明のポリカーボネート樹脂組成物に使用するポリカーボネート樹脂は、通常のポリカーボネート樹脂を製造するそれ自体公知の反応手段、例えばジオール成分に炭酸ジエステルなどのカーボネート前駆物質を反応させる方法により製造される。次にこれらの製造方法について基本的な手段を簡単に説明する。
<Production method of polycarbonate resin>
The polycarbonate resin used in the polycarbonate resin composition of the present invention is produced by a reaction means known per se for producing an ordinary polycarbonate resin, for example, a method of reacting a diol component with a carbonate precursor such as a carbonic acid diester. Next, basic means for these manufacturing methods will be briefly described.
カーボネート前駆物質として炭酸ジエステルを用いるエステル交換反応は、不活性ガス雰囲気下所定割合の芳香族ジヒドロキシ成分を炭酸ジエステルと加熱しながら撹拌して、生成するアルコールまたはフェノール類を留出させる方法により行われる。反応温度は生成するアルコールまたはフェノール類の沸点などにより異なるが、通常120〜300℃の範囲である。反応はその初期から減圧にして生成するアルコールまたはフェノール類を留出させながら反応を完結させる。また、必要に応じて末端停止剤、酸化防止剤等を加えてもよい。 The transesterification reaction using a carbonic acid diester as a carbonate precursor is performed by a method in which an aromatic dihydroxy component in a predetermined ratio is stirred with a carbonic acid diester while heating with an inert gas atmosphere to distill the generated alcohol or phenols. . The reaction temperature varies depending on the boiling point of the alcohol or phenol produced, but is usually in the range of 120 to 300 ° C. The reaction is completed while distilling off the alcohol or phenol produced under reduced pressure from the beginning. Moreover, you may add a terminal stopper, antioxidant, etc. as needed.
前記エステル交換反応に使用される炭酸ジエステルとしては、置換されてもよい炭素数6〜12のアリール基、アラルキル基等のエステルが挙げられる。具体的には、ジフェニルカーボネート、ジトリールカーボネート、ビス(クロロフェニル)カーボネートおよびm−クレジルカーボネート等が例示される。なかでもジフェニルカーボネートが特に好ましい。ジフェニルカーボネートの使用量は、ジヒドロキシ化合物の合計1モルに対して、好ましくは0.90〜1.02モル、より好ましは0.95〜1.00モルである。 Examples of the carbonic acid diester used in the transesterification include esters such as an aryl group having 6 to 12 carbon atoms and an aralkyl group which may be substituted. Specific examples include diphenyl carbonate, ditolyl carbonate, bis (chlorophenyl) carbonate and m-cresyl carbonate. Of these, diphenyl carbonate is particularly preferred. The amount of diphenyl carbonate to be used is preferably 0.90 to 1.02 mol, more preferably 0.95 to 1.00 mol, based on 1 mol of the total of dihydroxy compounds.
また溶融重合法においては重合速度を速めるために、重合触媒を用いることができ、かかる重合触媒としては、アルカリ金属化合物、アルカリ土類金属化合物、塩基性リン化合物、含窒素化合物、金属化合物等が挙げられる。このような化合物としては、アルカリ金属やアルカリ土類金属の、有機酸塩、無機塩、酸化物、水酸化物、水素化物、アルコキシド、4級アンモニウムヒドロキシド等が好ましく用いられ、これらの化合物は単独もしくは組み合わせて用いることができる。 In the melt polymerization method, a polymerization catalyst can be used to increase the polymerization rate. Examples of the polymerization catalyst include alkali metal compounds, alkaline earth metal compounds, basic phosphorus compounds, nitrogen-containing compounds, and metal compounds. Can be mentioned. As such compounds, organic acid salts, inorganic salts, oxides, hydroxides, hydrides, alkoxides, quaternary ammonium hydroxides, and the like of alkali metals and alkaline earth metals are preferably used. It can be used alone or in combination.
アルカリ金属化合物としては、水酸化ナトリウム、水酸化カリウム、水酸化セシウム、水酸化リチウム、炭酸水素ナトリウム、炭酸ナトリウム、炭酸カリウム、炭酸セシウム、炭酸リチウム、酢酸ナトリウム、酢酸カリウム、酢酸セシウム、酢酸リチウム、ステアリン酸ナトリウム、ステアリン酸カリウム、ステアリン酸セシウム、ステアリン酸リチウム、水素化ホウ素ナトリウム、安息香酸ナトリウム、安息香酸カリウム、安息香酸セシウム、安息香酸リチウム、リン酸水素2ナトリウム、リン酸水素2カリウム、リン酸水素2リチウム、フェニルリン酸2ナトリウム、ビスフェノールAの2ナトリウム塩、2カリウム塩、2セシウム塩、2リチウム塩、フェノールのナトリウム塩、カリウム塩、セシウム塩、リチウム塩等が例示される。 Examples of the alkali metal compound include sodium hydroxide, potassium hydroxide, cesium hydroxide, lithium hydroxide, sodium bicarbonate, sodium carbonate, potassium carbonate, cesium carbonate, lithium carbonate, sodium acetate, potassium acetate, cesium acetate, lithium acetate, Sodium stearate, potassium stearate, cesium stearate, lithium stearate, sodium borohydride, sodium benzoate, potassium benzoate, cesium benzoate, lithium benzoate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, phosphorus Examples include dilithium oxyhydrogen, disodium phenylphosphate, disodium salt of bisphenol A, 2 potassium salt, 2 cesium salt, 2 lithium salt, sodium salt of phenol, potassium salt, cesium salt, lithium salt and the like.
アルカリ土類金属化合物としては、水酸化マグネシウム、水酸化カルシウム、水酸化ストロンチウム、水酸化バリウム、炭酸マグネシウム、炭酸カルシウム、炭酸ストロンチウム、炭酸バリウム、炭酸水素カルシウム、炭酸水素バリウム、炭酸水素マグネシウム、炭酸水素ストロンチウム、二酢酸マグネシウム、二酢酸カルシウム、二酢酸ストロンチウム、二酢酸バリウム等が例示される。塩基性ホウ素化合物としては、例えば、テトラメチルホウ素、テトラエチルホウ素、テトラプロピルホウ素、テトラブチルホウ素、トリメチルエチルホウ素、トリメチルベンジルホウ素、トリメチルフェニルホウ素、トリエチルメチルホウ素、トリエチルベンジルホウ素、トリエチルフェニルホウ素、トリブチルベンジルホウ素、トリブチルフェニルホウ素、テトラフェニルホウ素、ベンジルトリフェニルホウ素、メチルトリフェニルホウ素、ブチルトリフェニルホウ素等のナトリウム塩、カリウム塩、リチウム塩、カルシウム塩、バリウム塩、マグネシウム塩、あるいはストロンチウム塩等が挙げられる。
塩基性リン化合物としては、例えば、トリエチルホスフィン、トリ−n−プロピルホスフィン、トリイソプロピルホスフィン、トリ−n−ブチルホスフィン、トリフェニルホスフィン、トリブチルホスフィン、あるいは四級ホスホニウム塩等が挙げられる。
Alkaline earth metal compounds include magnesium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide, magnesium carbonate, calcium carbonate, strontium carbonate, barium carbonate, calcium bicarbonate, barium bicarbonate, magnesium bicarbonate, bicarbonate Examples include strontium, magnesium diacetate, calcium diacetate, strontium diacetate, and barium diacetate. Examples of the basic boron compound include tetramethyl boron, tetraethyl boron, tetrapropyl boron, tetrabutyl boron, trimethylethyl boron, trimethylbenzyl boron, trimethylphenyl boron, triethylmethyl boron, triethylbenzyl boron, triethylphenyl boron, tributylbenzyl. Examples include sodium, potassium, lithium, calcium, barium, magnesium, or strontium salts such as boron, tributylphenylboron, tetraphenylboron, benzyltriphenylboron, methyltriphenylboron, butyltriphenylboron, etc. It is done.
Examples of the basic phosphorus compound include triethylphosphine, tri-n-propylphosphine, triisopropylphosphine, tri-n-butylphosphine, triphenylphosphine, tributylphosphine, and quaternary phosphonium salts.
含窒素化合物としては、テトラメチルアンモニウムヒドロキシド、テトラエチルアンモニウムヒドロキシド、テトラプロピルアンモニウムヒドロキシド、テトラブチルアンモニウムヒドロキシド、トリメチルベンジルアンモニウムヒドロキシド等のアルキル、アリール基等を有する4級アンモニウムヒドロキシド類が挙げられる。また、トリエチルアミン、ジメチルベンジルアミン、トリフェニルアミン等の3級アミン類、2−メチルイミダゾール、2−フェニルイミダゾール、ベンゾイミダゾール等のイミダゾール類が挙げられる。また、アンモニア、テトラメチルアンモニウムボロハイドライド、テトラブチルアンモニウムボロハイドライド、テトラブチルアンモニウムテトラフェニルボレート、テトラフェニルアンモニウムテトラフェニルボレート等の塩基あるいは塩基性塩等が例示される。金属化合物としては亜鉛アルミニウム化合物、ゲルマニウム化合物、有機スズ化合物、アンチモン化合物、マンガン化合物、チタン化合物、ジルコニウム化合物等が例示される。これらの化合物は1種または2種以上併用してもよい。 Examples of nitrogen-containing compounds include quaternary ammonium hydroxides having alkyl, aryl groups, etc., such as tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, and trimethylbenzylammonium hydroxide. Can be mentioned. Further, tertiary amines such as triethylamine, dimethylbenzylamine, and triphenylamine, and imidazoles such as 2-methylimidazole, 2-phenylimidazole, and benzimidazole can be used. Moreover, bases or basic salts such as ammonia, tetramethylammonium borohydride, tetrabutylammonium borohydride, tetrabutylammonium tetraphenylborate, tetraphenylammonium tetraphenylborate and the like are exemplified. Examples of metal compounds include zinc aluminum compounds, germanium compounds, organotin compounds, antimony compounds, manganese compounds, titanium compounds, zirconium compounds, and the like. These compounds may be used alone or in combination of two or more.
これらの重合触媒の使用量は、ジオール成分1モルに対し好ましくは1×10−9〜1×10−2当量、好ましくは1×10−8〜1×10−3当量、より好ましくは1×10−7〜1×10−5当量の範囲で選ばれる。
また、必要によって反応後期に触媒失活剤を添加してもよい。使用する触媒失活剤としては、公知の触媒失活剤が有効に使用されるが、この中でもスルホン酸のアンモニウム塩、ホスホニウム塩が好ましい。更にドデシルベンゼンスルホン酸テトラブチルホスホニウム塩等のドデシルベンゼンスルホン酸の塩類、パラトルエンスルホン酸テトラブチルアンモニウム塩等のパラトルエンスルホン酸の塩類が好ましい。
The amount of these polymerization catalysts used is preferably 1 × 10 −9 to 1 × 10 −2 equivalent, preferably 1 × 10 −8 to 1 × 10 −3 equivalent, more preferably 1 ×, relative to 1 mol of the diol component. It is selected in the range of 10 −7 to 1 × 10 −5 equivalents.
Further, if necessary, a catalyst deactivator may be added at a later stage of the reaction. As the catalyst deactivator to be used, a known catalyst deactivator is effectively used. Among them, sulfonic acid ammonium salt and phosphonium salt are preferable. Furthermore, salts of dodecylbenzenesulfonic acid such as tetrabutylphosphonium salt of dodecylbenzenesulfonic acid and salts of paratoluenesulfonic acid such as tetrabutylammonium salt of paratoluenesulfonic acid are preferable.
またスルホン酸のエステルとして、ベンゼンスルホン酸メチル、ベンゼンスルホン酸エチル、ベンゼンスルホン酸ブチル、ベンゼンスルホン酸オクチル、ベンゼンスルホン酸フェニル、パラトルエンスルホン酸メチル、パラトルエンスルホン酸エチル、パラトルエンスルホン酸ブチル、パラトルエンスルホン酸オクチル、パラトルエンスルホン酸フェニル等が好ましく用いられる。なかでも、ドデシルベンゼンスルホン酸テトラブチルホスホニウム塩が最も好ましく使用される。 Further, as esters of sulfonic acid, methyl benzenesulfonate, ethyl benzenesulfonate, butyl benzenesulfonate, octyl benzenesulfonate, phenyl benzenesulfonate, methyl paratoluenesulfonate, ethyl paratoluenesulfonate, butyl paratoluenesulfonate, Octyl paratoluenesulfonate, phenyl paratoluenesulfonate and the like are preferably used. Among these, dodecylbenzenesulfonic acid tetrabutylphosphonium salt is most preferably used.
これらの触媒失活剤の使用量はアルカリ金属化合物および/またはアルカリ土類金属化合物より選ばれた少なくとも1種の重合触媒を用いた場合、その触媒1モル当たり好ましくは0.5〜50モルの割合で、より好ましくは0.5〜10モルの割合で、更に好ましくは0.8〜5モルの割合で使用することができる。 The amount of the catalyst deactivator used is preferably 0.5 to 50 mol per mol of the catalyst when at least one polymerization catalyst selected from alkali metal compounds and / or alkaline earth metal compounds is used. It can be used in a proportion, more preferably in a proportion of 0.5 to 10 mol, still more preferably in a proportion of 0.8 to 5 mol.
また、本発明のポリカーボネート樹脂組成物は、用途や必要に応じて熱安定剤、可塑剤、光安定剤、重合金属不活性化剤、難燃剤、滑剤、帯電防止剤、界面活性剤、抗菌剤、紫外線吸収剤、離型剤等の添加剤を配合することができる。これらの添加剤は、混練を行う前にポリカーボネート樹脂(A)及び(B)の各々、もしくはどちらか一方に事前に添加しておいてもよいし、ブレンド混練り時に同時に添加して練りこんでも、混合後に練りこんでもよい。 In addition, the polycarbonate resin composition of the present invention includes a heat stabilizer, a plasticizer, a light stabilizer, a polymerized metal deactivator, a flame retardant, a lubricant, an antistatic agent, a surfactant, and an antibacterial agent as necessary and necessary. Additives such as ultraviolet absorbers and mold release agents can be blended. These additives may be added in advance to each or one of the polycarbonate resins (A) and (B) before kneading, or they may be added and kneaded at the same time during blend kneading. It may be kneaded after mixing.
〈ポリカーボネート樹脂組成物の製造方法〉
本発明のポリカーボネート樹脂組成物の製造方法は、特に制限はなく、例えば、
〔1〕ポリカーボネート樹脂(A)と(B)のそれぞれの固体を混合し、混練機により混練する方法、
〔2〕溶融状態の(A)に、固体の(B)を添加して混練する方法、
〔3〕溶融状態の(B)に、固体の(A)を添加して混練する方法、
〔4〕溶融状態の(A)と(B)の樹脂を混合して混練する方法、
のいずれの方法によって製造することもできる。混練は、連続式、バッチ式のどちらでもよい。混練機は、連続式ならば押出し機が好適であり、バッチ式ならばラボプラストミル、ニーダー好適に使用される。
本発明のポリカーボネート樹脂組成物の製造方法として、ポリカーボネート樹脂(A)と(B)を溶媒に溶解させ、鋳型に注ぎ込んだ後溶媒を蒸発させる方法がある。溶媒としては、メチレンクロライド、クロロホルム、クレゾールなどが使用される。
<Method for producing polycarbonate resin composition>
The production method of the polycarbonate resin composition of the present invention is not particularly limited, for example,
[1] A method of mixing each of the polycarbonate resins (A) and (B) and kneading them with a kneader,
[2] A method of adding and kneading solid (B) to molten (A),
[3] A method of adding and kneading solid (A) to molten (B),
[4] A method of mixing and kneading the molten resins (A) and (B),
It can be produced by any of the methods. The kneading may be either a continuous type or a batch type. The kneader is preferably an extruder if it is a continuous type, and is preferably used for a lab plast mill or a kneader if it is a batch type.
As a method for producing the polycarbonate resin composition of the present invention, there is a method in which the polycarbonate resins (A) and (B) are dissolved in a solvent, poured into a mold, and then the solvent is evaporated. As the solvent, methylene chloride, chloroform, cresol and the like are used.
〈光学部材〉
本発明のポリカーボネート樹脂組成物からなる光学部材は、射出成形、圧縮成形、射出圧縮成形、溶融押出成形、溶融押出製膜、キャスティング製膜等の任意の方法により成形、加工することができる。
本発明のポリカーボネート樹脂からなる光学部材とは、光ディスク、透明導電性基板、光カード、シート、フィルム、光ファイバー、レンズ、プリズム、光学膜、基盤、光学フィルター、ハードコート膜等である。
<Optical member>
The optical member made of the polycarbonate resin composition of the present invention can be molded and processed by any method such as injection molding, compression molding, injection compression molding, melt extrusion molding, melt extrusion film formation, casting film formation and the like.
The optical member made of the polycarbonate resin of the present invention includes an optical disk, a transparent conductive substrate, an optical card, a sheet, a film, an optical fiber, a lens, a prism, an optical film, a substrate, an optical filter, a hard coat film, and the like.
〈光学レンズ〉
本発明のポリカーボネート樹脂組成物からなる光学レンズは、射出成形、圧縮成形、射出圧縮成形、溶融押出成形、キャスティング等の任意の方法により成形、加工することができるが、射出成形が特に好適である。射出成形の成形条件は特に限定されないが、成形機のシリンダ温度は180〜320℃が好ましく、220〜300℃がより好ましく、260〜290℃がよりいっそう好ましい。また、金型温度は70〜150℃が好ましく、80〜140℃がより好ましく、90〜130℃がよりいっそう好ましい。射出圧力は100〜2,000kgf/cm2が好ましく、500〜1,700kgf/cm2が好ましく、700〜1,500kgf/cm2がよりいっそう好ましい。また、成形加工前に、本発明のポリカーボネート樹脂組成物を100〜130℃で1〜12時間事前乾燥することが好ましい。
<Optical lens>
The optical lens comprising the polycarbonate resin composition of the present invention can be molded and processed by any method such as injection molding, compression molding, injection compression molding, melt extrusion molding, casting, etc., but injection molding is particularly suitable. . The molding conditions for injection molding are not particularly limited, but the cylinder temperature of the molding machine is preferably 180 to 320 ° C, more preferably 220 to 300 ° C, and even more preferably 260 to 290 ° C. The mold temperature is preferably 70 to 150 ° C, more preferably 80 to 140 ° C, and still more preferably 90 to 130 ° C. Injection pressure is preferably 100~2,000kgf / cm 2, preferably 500~1,700kgf / cm 2, and still more preferably, 700~1,500kgf / cm 2. Moreover, it is preferable to pre-dry the polycarbonate resin composition of this invention for 1 to 12 hours at 100-130 degreeC before a shaping | molding process.
本発明のポリカーボネート樹脂組成物からなる光学レンズは、屈折率が高いことを特徴とする。一般的に、屈折率が高いと、同一屈折率を有するレンズエレメントをより曲率の小さい面で実現できるため、この面で発生する収差量を小さくできる。その結果、レンズの枚数を減らしたり、レンズの偏心感度を低減したり、レンズ厚みを薄くして軽量化することが可能になる。 An optical lens comprising the polycarbonate resin composition of the present invention is characterized by a high refractive index. In general, when the refractive index is high, a lens element having the same refractive index can be realized on a surface with a smaller curvature, so that the amount of aberration generated on this surface can be reduced. As a result, it is possible to reduce the number of lenses, reduce the decentration sensitivity of the lenses, or reduce the lens thickness to reduce the weight.
本発明のポリカーボネート樹脂組成物からなる光学レンズは、光学歪みが小さいことを特徴とする。一般的なビスフェノールAタイプのポリカーボネートからなる光学レンズは光学歪みが大きい。成形条件によりその値を低減することも不可能ではないが、その条件幅は非常に小さく成形が非常に困難となる。本発明の樹脂は、樹脂の配向により生じる光学歪みが極めて小さく、また成形歪みも小さいため、成形条件を厳密に設定しなくても良好な光学レンズを得ることができる。 The optical lens comprising the polycarbonate resin composition of the present invention is characterized by having a small optical distortion. An optical lens made of a general bisphenol A type polycarbonate has a large optical distortion. Although it is not impossible to reduce the value depending on molding conditions, the condition width is very small and molding becomes very difficult. Since the resin of the present invention has a very small optical strain caused by the orientation of the resin and a small molding strain, a good optical lens can be obtained without strictly setting molding conditions.
本発明のポリカーボネート樹脂組成物からなる光学レンズは、必要に応じて非球面レンズの形で用いることが好適に実施される。非球面レンズは、1枚のレンズで球面収差を実質的にゼロとすることが可能であるため、複数の球面レンズの組み合わせで球面収差を取り除く必要がなく、軽量化および生産コストの低減化が可能になる。従って、非球面レンズは、光学レンズの中でも特にカメラレンズとして有用である。 The optical lens made of the polycarbonate resin composition of the present invention is preferably used in the form of an aspheric lens as necessary. Since an aspheric lens can substantially eliminate spherical aberration with a single lens, there is no need to remove spherical aberration with a combination of a plurality of spherical lenses, thus reducing weight and reducing production costs. It becomes possible. Therefore, the aspherical lens is particularly useful as a camera lens among optical lenses.
また、本発明のポリカーボネート樹脂組成物は、流動性が高いため、薄肉小型で複雑な形状である光学レンズの材料として特に有用である。具体的なレンズサイズとして、中心部の厚みが0.05〜3.0mm、より好ましくは0.05〜2.0mm、さらに好ましくは0.1〜1.0mmである。また、直径が1.0mm〜20.0mm、より好ましくは1.0〜10.0mm、さらに好ましくは3.0〜10.0mmである。また、その形状として片面が凸、片面が凹であるメニスカスレンズであることが好ましい。 Moreover, since the polycarbonate resin composition of the present invention has high fluidity, it is particularly useful as a material for an optical lens having a thin and small size and a complicated shape. As a specific lens size, the thickness of the central portion is 0.05 to 3.0 mm, more preferably 0.05 to 2.0 mm, and still more preferably 0.1 to 1.0 mm. Moreover, a diameter is 1.0 mm-20.0 mm, More preferably, it is 1.0-10.0 mm, More preferably, it is 3.0-10.0 mm. In addition, it is preferably a meniscus lens having a convex surface on one side and a concave surface on the other side.
本発明のポリカーボネート樹脂組成物からなる光学レンズの表面には、必要に応じ、反射防止層あるいはハードコート層といったコート層が設けられていても良い。反射防止層は、単層であっても多層であっても良く、有機物であっても無機物であっても構わないが、無機物であることが好ましい。具体的には、酸化ケイ素、酸化アルミニウム、酸化ジルコニウム、酸化チタニウム、酸化セリウム、酸化マグネシウム、フッ化マグネシウム等の酸化物あるいはフッ化物が例示される。
また、本発明のポリカーボネート樹脂組成物からなる光学レンズは、金型成形、切削、研磨、レーザー加工、放電加工、エッジングなど任意の方法により成形されてもよい。さらには、金型成形がより好ましい。
On the surface of the optical lens made of the polycarbonate resin composition of the present invention, a coating layer such as an antireflection layer or a hard coating layer may be provided as necessary. The antireflection layer may be a single layer or a multilayer, and may be organic or inorganic, but is preferably inorganic. Specific examples include oxides or fluorides such as silicon oxide, aluminum oxide, zirconium oxide, titanium oxide, cerium oxide, magnesium oxide, and magnesium fluoride.
In addition, the optical lens made of the polycarbonate resin composition of the present invention may be molded by any method such as mold molding, cutting, polishing, laser processing, electric discharge processing, and edging. Furthermore, mold molding is more preferable.
〈透明フィルム〉
本発明のポリカーボネート樹脂組成物からなる透明フィルムは、溶融押出製膜、キャスト製膜等の任意の方法により成形、加工することができる。
本発明のポリカーボネート樹脂組成物からなる透明フィルムとは、ディスプレイ用フィルム、延伸フィルム、加飾フィルム等である。
溶融押出製膜においては、Tダイを用いて樹脂を押し出し冷却ロールに送る方法が好ましく用いられる。押出機のシリンダ温度は、180〜320℃が好ましく、200℃〜300℃の範囲がより好ましい。また、成形加工前に、本発明のポリカーボネート樹脂組成物を100〜130℃で1〜12時間事前乾燥することが好ましい。
<Transparent film>
The transparent film comprising the polycarbonate resin composition of the present invention can be molded and processed by any method such as melt extrusion film formation or cast film formation.
The transparent film made of the polycarbonate resin composition of the present invention includes a display film, a stretched film, a decorative film, and the like.
In melt extrusion film formation, a method in which a resin is extruded using a T die and sent to a cooling roll is preferably used. The cylinder temperature of the extruder is preferably 180 to 320 ° C, and more preferably 200 to 300 ° C. Moreover, it is preferable to pre-dry the polycarbonate resin composition of this invention for 1 to 12 hours at 100-130 degreeC before a shaping | molding process.
本発明で用いるポリカーボネート樹脂は、有機溶媒に対する溶解性が良好なので、溶液キャスト製膜も適用することが出来る。溶媒としては塩化メチレン、1,2−ジクロロエタン、1,1,2,2−テトラクロロエタン、ジオキソラン、ジオキサン等が好適に用いられる。
本発明のポリカーボネート樹脂組成物からなる透明フィルムの厚みは、30〜500μmの範囲が好ましく、より好ましくは40〜400μmの範囲である。
Since the polycarbonate resin used in the present invention has good solubility in organic solvents, solution cast film formation can also be applied. As the solvent, methylene chloride, 1,2-dichloroethane, 1,1,2,2-tetrachloroethane, dioxolane, dioxane and the like are preferably used.
The thickness of the transparent film made of the polycarbonate resin composition of the present invention is preferably in the range of 30 to 500 μm, more preferably in the range of 40 to 400 μm.
以下に実施例を挙げて本発明をさらに説明する。
実施例1〜4、比較例1〜2
評価用サンプルは以下の方法で調製した。
(a)フィルム
得られた樹脂組成物3gを塩化メチレン50mlに溶解させ、ガラスシャーレ上にキャストする。室温にて十分に乾燥させた後、120℃以下の温度にて8時間乾燥して、厚さ約100μmのキャストフィルムを作成した。
The following examples further illustrate the present invention.
Examples 1-4, Comparative Examples 1-2
An evaluation sample was prepared by the following method.
(A) Film 3 g of the obtained resin composition is dissolved in 50 ml of methylene chloride and cast on a glass petri dish. After sufficiently drying at room temperature, it was dried at a temperature of 120 ° C. or lower for 8 hours to prepare a cast film having a thickness of about 100 μm.
評価は下記の方法によった。
(1)比粘度:得られた樹脂組成物を十分に乾燥し、該樹脂0.7gを塩化メチレン100mlに溶解した溶液から、その溶液の20℃における比粘度(ηsp)を測定した。
(2)屈折率(nd)、アッベ数(ν):(a)の手法により作成したフィルムをATAGO製DR−M2のアッベ屈折計を用いて、25℃における屈折率(波長:589nm)及びアッベ数を測定した。
(3)配向複屈折:(a)の手法により作成したフィルムを長さ7cm、幅1.5cmにカットした後、長手方向の両端をチャックに挟み(チャック間4.5cm)、ポリカーボネート樹脂のTg+10℃で2倍延伸し、日本分光(株)製エリプソメーターM−220を用いて589nmにおける位相差(Re)を測定し、下記式より配向複屈折(Δn)を求めた。
Δn=Re/d
Δn:配向複屈折
Re:位相差
d:厚さ
(4)耐折り曲げ性:(a)の手法により作成したフィルムから長さ40mm、幅10mmの長方形の試験片を切り出した。万力の左右の接合面の間隔を40mmに開き、前記試験片の両端を接合面内に固定した。次に左右の接合面の間隔を2mm/秒以下の速度で狭めていき、折れ曲がった試験片全体を該接合面内で圧縮した。そして、接合面間が完全に密着する迄に試験片が折れ曲がり部で2片(又は3片以上の破片)に割れた際、万力の接合面の移動を停止し、接合面の間隔を測定した。
(5)鉛筆硬度:(a)の手法により作成したフィルムをJIS K5600−5−4に準拠し、750g加重で鉛筆硬度の測定を行い、表面に目視で傷がつかなかった鉛筆の硬度を評価結果とした。鉛筆は三菱鉛筆Uni(商品名)を使用した。
Evaluation was based on the following method.
(1) Specific viscosity: The obtained resin composition was sufficiently dried, and the specific viscosity (η sp ) at 20 ° C. of the solution was measured from a solution obtained by dissolving 0.7 g of the resin in 100 ml of methylene chloride.
(2) Refractive index (nd), Abbe number (ν): A film prepared by the method of (a) was measured with a refractive index (wavelength: 589 nm) and Abbe at 25 ° C. using an Abbe refractometer manufactured by ATAGO DR-M2. Number was measured.
(3) Oriented birefringence: after the film prepared by the method of (a) is cut into a length of 7 cm and a width of 1.5 cm, both ends in the longitudinal direction are sandwiched between chucks (4.5 cm between chucks), and Tg + 10 of polycarbonate resin The film was stretched twice at 0 ° C., the phase difference (Re) at 589 nm was measured using an ellipsometer M-220 manufactured by JASCO Corporation, and the orientation birefringence (Δn) was determined from the following formula.
Δn = Re / d
Δn: orientation birefringence
Re: Phase difference
d: Thickness (4) Bending resistance: A rectangular test piece having a length of 40 mm and a width of 10 mm was cut out from the film prepared by the method of (a). The space between the left and right joint surfaces of the vise was opened to 40 mm, and both ends of the test piece were fixed in the joint surface. Next, the interval between the left and right joint surfaces was narrowed at a speed of 2 mm / second or less, and the entire bent test piece was compressed in the joint surface. And when the test piece is bent into two pieces (or more than three pieces) at the bent part until the joint surfaces are completely in close contact, the movement of the joint surface of the vise is stopped and the distance between the joint surfaces is measured. did.
(5) Pencil hardness: The film prepared by the method of (a) is measured in accordance with JIS K5600-5-4, the pencil hardness is measured with a weight of 750 g, and the hardness of the pencil that is not visually scratched on the surface is evaluated. As a result. The pencil used was Mitsubishi Pencil Uni (trade name).
(ポリカーボネート樹脂の重合)
参考例1(ポリカーボネート樹脂(A)の製造)
9,9−ビス[4−(2−ヒドロキシエトキシ)−3−フェニルフェニル]フルオレン(以下“OPBPEF”と省略することがある)177.21部、ジフェニルカーボネート(以下“DPC”と省略することがある)63.62部、及び水酸化ナトリウム0.012×10−3部を攪拌機および留出装置付きの反応釜に入れ、窒素置換を3度行った後、ジャケットを180℃に加熱し、原料を溶融させた。完全溶解後、20分かけて20kPaまで減圧すると同時に、60℃/hrの速度でジャケットを260℃まで昇温し、エステル交換反応を行った。その後、ジャケットを260℃に保持したまま、80分かけて0.13kPaまで減圧し、260℃、0.13kPa以下の条件下で5〜30分重合反応を行った。反応終了後、生成したポリカーボネート樹脂をペレタイズしながら抜き出し、ポリカーボネート樹脂ペレットを得た。
(Polymer resin polymerization)
Reference Example 1 (Production of polycarbonate resin (A))
17,7.21 parts of 9,9-bis [4- (2-hydroxyethoxy) -3-phenylphenyl] fluorene (hereinafter sometimes abbreviated as “OPBPEF”), diphenyl carbonate (hereinafter abbreviated as “DPC”) A) 63.62 parts and 0.012 × 10 −3 parts of sodium hydroxide were placed in a reactor equipped with a stirrer and a distillation apparatus, and after replacing with nitrogen three times, the jacket was heated to 180 ° C. Was melted. After complete dissolution, the pressure was reduced to 20 kPa over 20 minutes, and at the same time, the jacket was heated to 260 ° C. at a rate of 60 ° C./hr to conduct a transesterification reaction. Thereafter, the pressure was reduced to 0.13 kPa over 80 minutes while maintaining the jacket at 260 ° C., and a polymerization reaction was performed for 5 to 30 minutes under the conditions of 260 ° C. and 0.13 kPa or less. After completion of the reaction, the produced polycarbonate resin was extracted while pelletizing to obtain polycarbonate resin pellets.
参考例2(ポリカーボネート樹脂(B)の製造)
OPBPEFを9,9−ビス(4−(2−ヒドロキシエトキシ)フェニル)フルオレン(以下“BPEF”と省略することがある)に変更し、131.55部とする以外は、実施例1と同様の方法でポリカーボネート樹脂ペレットを得た。
Reference Example 2 (Production of polycarbonate resin (B))
The same as in Example 1 except that OPBPEF was changed to 9,9-bis (4- (2-hydroxyethoxy) phenyl) fluorene (hereinafter sometimes abbreviated as “BPEF”) to 131.55 parts. Polycarbonate resin pellets were obtained by this method.
(ポリカーボネート樹脂組成物の製造)
実施例1
参考例で作成したポリカーボネート樹脂(A)及び(B)を表1の割合で使用し、さらに、ポリカーボネート樹脂(A)及び(B)の合計100重量部に対して、BASF製IRGAFOS168を0.05重量部、理研ビタミン(株)製リケマールS−100Aを0.1重量部加えてよく振り混ぜた後、ベント付きφ30mm二軸押出機を用いて混練し、ポリカーボネート樹脂組成物のペレットを得た。該ペレットを用いて、比粘度、屈折率、配向複屈折、耐折り曲げ性、鉛筆硬度を測定し、結果を表1に記載した。
(Manufacture of polycarbonate resin composition)
Example 1
The polycarbonate resins (A) and (B) prepared in the reference examples were used in the ratios shown in Table 1, and 0.05% of BASF IRGAFOS168 was added to 100 parts by weight of the polycarbonate resins (A) and (B). Part by weight, 0.1 part by weight of Riken Vitamin Co., Ltd. Riquemar S-100A was added and well shaken, and then kneaded using a vented φ30 mm twin screw extruder to obtain a pellet of a polycarbonate resin composition. Using the pellets, specific viscosity, refractive index, orientation birefringence, bending resistance, and pencil hardness were measured, and the results are shown in Table 1.
実施例2
参考例で作成したポリカーボネート樹脂(A)及び(B)を表1の割合で使用する以外は、実施例1と同様の方法でポリカーボネート樹脂組成物のペレットを得た。該ペレットを用いて、比粘度、屈折率、配向複屈折、耐折り曲げ性、鉛筆硬度を測定し、結果を表1に記載した。
Example 2
A pellet of the polycarbonate resin composition was obtained in the same manner as in Example 1 except that the polycarbonate resins (A) and (B) prepared in Reference Example were used in the proportions shown in Table 1. Using the pellets, specific viscosity, refractive index, orientation birefringence, bending resistance, and pencil hardness were measured, and the results are shown in Table 1.
実施例3
参考例で作成したポリカーボネート樹脂(A)及び(B)を表1の割合で使用する以外は、実施例1と同様の方法でポリカーボネート樹脂組成物のペレットを得た。該ペレットを用いて、比粘度、屈折率、配向複屈折、耐折り曲げ性、鉛筆硬度を測定し、結果を表1に記載した。
Example 3
A pellet of the polycarbonate resin composition was obtained in the same manner as in Example 1 except that the polycarbonate resins (A) and (B) prepared in Reference Example were used in the proportions shown in Table 1. Using the pellets, specific viscosity, refractive index, orientation birefringence, bending resistance, and pencil hardness were measured, and the results are shown in Table 1.
実施例4
参考例で作成したポリカーボネート樹脂(A)及び(B)を表1の割合で使用する以外は、実施例1と同様の方法でポリカーボネート樹脂組成物のペレットを得た。該ペレットを用いて、比粘度、屈折率、配向複屈折、耐折り曲げ性、鉛筆硬度を測定し、結果を表1に記載した。
Example 4
A pellet of the polycarbonate resin composition was obtained in the same manner as in Example 1 except that the polycarbonate resins (A) and (B) prepared in Reference Example were used in the proportions shown in Table 1. Using the pellets, specific viscosity, refractive index, orientation birefringence, bending resistance, and pencil hardness were measured, and the results are shown in Table 1.
比較例1
参考例で作成したポリカーボネート樹脂(A)のみを使用する以外は、実施例1と同様の方法でポリカーボネート樹脂組成物のペレットを得た。該ペレットを用いて、比粘度、屈折率、配向複屈折、耐折り曲げ性、鉛筆硬度を測定し、結果を表1に記載した。
Comparative Example 1
A pellet of the polycarbonate resin composition was obtained in the same manner as in Example 1 except that only the polycarbonate resin (A) prepared in the reference example was used. Using the pellets, specific viscosity, refractive index, orientation birefringence, bending resistance, and pencil hardness were measured, and the results are shown in Table 1.
比較例2
参考例で作成したポリカーボネート樹脂(B)のみを使用する以外は、実施例1と同様の方法でポリカーボネート樹脂組成物のペレットを得た。該ペレットを用いて、比粘度、屈折率、配向複屈折、耐折り曲げ性、鉛筆硬度を測定し、結果を表1に記載した。
Comparative Example 2
A pellet of the polycarbonate resin composition was obtained in the same manner as in Example 1 except that only the polycarbonate resin (B) prepared in the reference example was used. Using the pellets, specific viscosity, refractive index, orientation birefringence, bending resistance, and pencil hardness were measured, and the results are shown in Table 1.
(光学レンズの成形)
作成したポリカーボネート樹脂組成物を120℃で8時間乾燥した後、住友重機械(株)製SE30DU射出成形機を用いて、成形温度290℃、金型温度140℃にて、厚さ0.3mm、凸面曲率半径5mm、凹面曲率半径4mm、φ5mmの光学レンズを射出成形した。評価は、500ショット成形した際に、成形片、スプルー、ランナーが折れ、金型に樹脂が残ってしまう等で連続成形を止めた回数を評価し、結果を表1に記載した。
(Molding optical lenses)
After the prepared polycarbonate resin composition was dried at 120 ° C. for 8 hours, using a SE30DU injection molding machine manufactured by Sumitomo Heavy Industries, Ltd., at a molding temperature of 290 ° C. and a mold temperature of 140 ° C., a thickness of 0.3 mm, An optical lens having a convex curvature radius of 5 mm, a concave curvature radius of 4 mm, and φ5 mm was injection molded. The evaluation was carried out by evaluating the number of times that continuous molding was stopped because the molded piece, sprue, and runner were broken when 500 shots were molded and the resin remained in the mold, and the results are shown in Table 1.
実施例1〜4で得られたポリカーボネート樹脂は、高屈折率、低複屈折であり、かつ、表面硬度と耐折り曲げ性のバランスに優れる。また、連続成形性も良い。これに対して、比較例1で得られたポリカーボネート樹脂は、脆いため、耐折り曲げ性及び連続成形性に劣る。また、比較例2で得られたポリカーボネート樹脂は、屈折率及び鉛筆硬度に劣る。 The polycarbonate resins obtained in Examples 1 to 4 have a high refractive index and low birefringence, and are excellent in balance between surface hardness and bending resistance. Moreover, continuous moldability is also good. On the other hand, the polycarbonate resin obtained in Comparative Example 1 is inferior in bending resistance and continuous moldability because it is brittle. Moreover, the polycarbonate resin obtained in Comparative Example 2 is inferior in refractive index and pencil hardness.
本発明のポリカーボネート樹脂は、光ディスク、透明導電性基板、光カード、シート、フィルム、光ファイバー、レンズ、プリズム、光学膜、基盤、光学フィルター、ハードコート膜等の光学部材に用いることができ極めて有用である。 The polycarbonate resin of the present invention can be used for optical members such as optical disks, transparent conductive substrates, optical cards, sheets, films, optical fibers, lenses, prisms, optical films, substrates, optical filters, and hard coat films, and is extremely useful. is there.
1.作業台
2.万力
21.取付基部
22.上取付部
23.下取付部
231.取付雌ネジ
232.取付ネジ軸
233.ハンドル
234.挟持板
24.固定口金
241.試験片設置用治具
242.挟持雌ネジ
243.接合面
25.可動口金
251.試験片設置用治具
252.シャフト
253.ハンドル
254.接合面
3.試験片
1. Working table 2.
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