JP2001216682A - Polycarbonate resin optical molding material having high definition transfer property and optical disk substrate formed from that material - Google Patents
Polycarbonate resin optical molding material having high definition transfer property and optical disk substrate formed from that materialInfo
- Publication number
- JP2001216682A JP2001216682A JP2000025269A JP2000025269A JP2001216682A JP 2001216682 A JP2001216682 A JP 2001216682A JP 2000025269 A JP2000025269 A JP 2000025269A JP 2000025269 A JP2000025269 A JP 2000025269A JP 2001216682 A JP2001216682 A JP 2001216682A
- Authority
- JP
- Japan
- Prior art keywords
- polycarbonate resin
- molecular weight
- bis
- weight
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229920005668 polycarbonate resin Polymers 0.000 title claims abstract description 58
- 239000004431 polycarbonate resin Substances 0.000 title claims abstract description 58
- 230000003287 optical effect Effects 0.000 title claims abstract description 23
- 239000012778 molding material Substances 0.000 title claims abstract description 9
- 239000000758 substrate Substances 0.000 title claims description 17
- 239000000463 material Substances 0.000 title description 8
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 15
- 239000004417 polycarbonate Substances 0.000 claims abstract description 15
- 238000005227 gel permeation chromatography Methods 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 31
- 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 claims description 24
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 20
- 125000003118 aryl group Chemical group 0.000 claims description 7
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 abstract description 24
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 abstract 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 54
- 239000000243 solution Substances 0.000 description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 24
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- -1 4,4 ′ -Dihydroxydiphenyl sulphoxide Chemical compound 0.000 description 13
- 239000000203 mixture Substances 0.000 description 13
- 238000003756 stirring Methods 0.000 description 11
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 10
- 150000002989 phenols Chemical class 0.000 description 10
- 238000006116 polymerization reaction Methods 0.000 description 10
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 9
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 239000011347 resin Substances 0.000 description 8
- 238000001746 injection moulding Methods 0.000 description 7
- 239000001294 propane Substances 0.000 description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 6
- 238000012695 Interfacial polymerization Methods 0.000 description 6
- 239000004793 Polystyrene Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- 229920002223 polystyrene Polymers 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- QHPQWRBYOIRBIT-UHFFFAOYSA-N 4-tert-butylphenol Chemical compound CC(C)(C)C1=CC=C(O)C=C1 QHPQWRBYOIRBIT-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 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
- 238000001914 filtration Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 238000007664 blowing Methods 0.000 description 4
- GRWZHXKQBITJKP-UHFFFAOYSA-L dithionite(2-) Chemical compound [O-]S(=O)S([O-])=O GRWZHXKQBITJKP-UHFFFAOYSA-L 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- ZIRIVHVGOAIFRG-UHFFFAOYSA-N methyl 2-(2-carboxyoxyphenyl)benzoate Chemical compound COC(=O)C1=CC=CC=C1C1=CC=CC=C1OC(O)=O ZIRIVHVGOAIFRG-UHFFFAOYSA-N 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 239000002685 polymerization catalyst Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 2
- GJYCVCVHRSWLNY-UHFFFAOYSA-N 2-butylphenol Chemical compound CCCCC1=CC=CC=C1O GJYCVCVHRSWLNY-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
- WJZHBPSXJJQGJO-UHFFFAOYSA-N 4-[2,6-di(propan-2-yl)phenyl]phenol Chemical compound CC(C)C1=CC=CC(C(C)C)=C1C1=CC=C(O)C=C1 WJZHBPSXJJQGJO-UHFFFAOYSA-N 0.000 description 2
- VGFSOACUVJLBAA-UHFFFAOYSA-N 4-[2-(4-hydroxyphenyl)-3,3-dimethylbutan-2-yl]phenol Chemical compound C=1C=C(O)C=CC=1C(C)(C(C)(C)C)C1=CC=C(O)C=C1 VGFSOACUVJLBAA-UHFFFAOYSA-N 0.000 description 2
- KANXFMWQMYCHHH-UHFFFAOYSA-N 4-[2-(4-hydroxyphenyl)-3-methylbutan-2-yl]phenol Chemical compound C=1C=C(O)C=CC=1C(C)(C(C)C)C1=CC=C(O)C=C1 KANXFMWQMYCHHH-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
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 2
- HTVITOHKHWFJKO-UHFFFAOYSA-N Bisphenol B Chemical compound C=1C=C(O)C=CC=1C(C)(CC)C1=CC=C(O)C=C1 HTVITOHKHWFJKO-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- MUCRFDZUHPMASM-UHFFFAOYSA-N bis(2-chlorophenyl) carbonate Chemical compound ClC1=CC=CC=C1OC(=O)OC1=CC=CC=C1Cl MUCRFDZUHPMASM-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 238000005809 transesterification reaction Methods 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- LKKLDKBWCWESPV-UHFFFAOYSA-N (2-phenylphenyl) hydrogen carbonate Chemical compound OC(=O)OC1=CC=CC=C1C1=CC=CC=C1 LKKLDKBWCWESPV-UHFFFAOYSA-N 0.000 description 1
- OBMAJDVACJRVJY-UHFFFAOYSA-N (3-bromo-2-phenylphenyl) hydrogen carbonate Chemical compound OC(=O)OC1=CC=CC(Br)=C1C1=CC=CC=C1 OBMAJDVACJRVJY-UHFFFAOYSA-N 0.000 description 1
- DQAROJXYWZUVDH-UHFFFAOYSA-N (3-chloro-2-phenylphenyl) hydrogen carbonate Chemical compound OC(=O)OC1=CC=CC(Cl)=C1C1=CC=CC=C1 DQAROJXYWZUVDH-UHFFFAOYSA-N 0.000 description 1
- JOSARTKEJSZAIX-UHFFFAOYSA-N (3-nitro-2-phenylphenyl) hydrogen carbonate Chemical compound OC(=O)OC1=CC=CC([N+]([O-])=O)=C1C1=CC=CC=C1 JOSARTKEJSZAIX-UHFFFAOYSA-N 0.000 description 1
- HCNHNBLSNVSJTJ-UHFFFAOYSA-N 1,1-Bis(4-hydroxyphenyl)ethane Chemical compound C=1C=C(O)C=CC=1C(C)C1=CC=C(O)C=C1 HCNHNBLSNVSJTJ-UHFFFAOYSA-N 0.000 description 1
- NFAOATPOYUWEHM-UHFFFAOYSA-N 2-(6-methylheptyl)phenol Chemical compound CC(C)CCCCCC1=CC=CC=C1O NFAOATPOYUWEHM-UHFFFAOYSA-N 0.000 description 1
- FDIPWBUDOCPIMH-UHFFFAOYSA-N 2-decylphenol Chemical compound CCCCCCCCCCC1=CC=CC=C1O FDIPWBUDOCPIMH-UHFFFAOYSA-N 0.000 description 1
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 description 1
- HMWIHOZPGQRZLR-UHFFFAOYSA-N 2-hexadecylphenol Chemical compound CCCCCCCCCCCCCCCCC1=CC=CC=C1O HMWIHOZPGQRZLR-UHFFFAOYSA-N 0.000 description 1
- QEMHBAGGYKJNSS-UHFFFAOYSA-N 2-icosylphenol Chemical compound CCCCCCCCCCCCCCCCCCCCC1=CC=CC=C1O QEMHBAGGYKJNSS-UHFFFAOYSA-N 0.000 description 1
- WCRKLZYTQVZTMM-UHFFFAOYSA-N 2-octadecylphenol Chemical compound CCCCCCCCCCCCCCCCCCC1=CC=CC=C1O WCRKLZYTQVZTMM-UHFFFAOYSA-N 0.000 description 1
- JOONSONEBWTBLT-UHFFFAOYSA-N 2-tetradecylphenol Chemical compound CCCCCCCCCCCCCCC1=CC=CC=C1O JOONSONEBWTBLT-UHFFFAOYSA-N 0.000 description 1
- RXNYJUSEXLAVNQ-UHFFFAOYSA-N 4,4'-Dihydroxybenzophenone Chemical compound C1=CC(O)=CC=C1C(=O)C1=CC=C(O)C=C1 RXNYJUSEXLAVNQ-UHFFFAOYSA-N 0.000 description 1
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 1
- VWGKEVWFBOUAND-UHFFFAOYSA-N 4,4'-thiodiphenol Chemical compound C1=CC(O)=CC=C1SC1=CC=C(O)C=C1 VWGKEVWFBOUAND-UHFFFAOYSA-N 0.000 description 1
- NZGQHKSLKRFZFL-UHFFFAOYSA-N 4-(4-hydroxyphenoxy)phenol Chemical compound C1=CC(O)=CC=C1OC1=CC=C(O)C=C1 NZGQHKSLKRFZFL-UHFFFAOYSA-N 0.000 description 1
- UJCYBTZHUJWCMB-UHFFFAOYSA-N 4-[1-(4-hydroxyphenyl)-4-propan-2-ylcyclohexyl]phenol Chemical compound C1CC(C(C)C)CCC1(C=1C=CC(O)=CC=1)C1=CC=C(O)C=C1 UJCYBTZHUJWCMB-UHFFFAOYSA-N 0.000 description 1
- ZBMWIKZBITYTCF-UHFFFAOYSA-N 4-[2,3-di(propan-2-yl)phenyl]phenol Chemical compound CC(C)C1=CC=CC(C=2C=CC(O)=CC=2)=C1C(C)C ZBMWIKZBITYTCF-UHFFFAOYSA-N 0.000 description 1
- VHLLJTHDWPAQEM-UHFFFAOYSA-N 4-[2-(4-hydroxyphenyl)-4-methylpentan-2-yl]phenol Chemical compound C=1C=C(O)C=CC=1C(C)(CC(C)C)C1=CC=C(O)C=C1 VHLLJTHDWPAQEM-UHFFFAOYSA-N 0.000 description 1
- WCUDAIJOADOKAW-UHFFFAOYSA-N 4-[2-(4-hydroxyphenyl)pentan-2-yl]phenol Chemical compound C=1C=C(O)C=CC=1C(C)(CCC)C1=CC=C(O)C=C1 WCUDAIJOADOKAW-UHFFFAOYSA-N 0.000 description 1
- NIRYBKWMEWFDPM-UHFFFAOYSA-N 4-[3-(4-hydroxyphenyl)-3-methylbutyl]phenol Chemical compound C=1C=C(O)C=CC=1C(C)(C)CCC1=CC=C(O)C=C1 NIRYBKWMEWFDPM-UHFFFAOYSA-N 0.000 description 1
- ZJNKCNFBTBFNMO-UHFFFAOYSA-N 4-[3-(4-hydroxyphenyl)-5,7-dimethyl-1-adamantyl]phenol Chemical compound C1C(C)(C2)CC(C3)(C)CC1(C=1C=CC(O)=CC=1)CC23C1=CC=C(O)C=C1 ZJNKCNFBTBFNMO-UHFFFAOYSA-N 0.000 description 1
- YWFPGFJLYRKYJZ-UHFFFAOYSA-N 9,9-bis(4-hydroxyphenyl)fluorene Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C2=CC=CC=C21 YWFPGFJLYRKYJZ-UHFFFAOYSA-N 0.000 description 1
- 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 1
- GIXXQTYGFOHYPT-UHFFFAOYSA-N Bisphenol P Chemical compound C=1C=C(C(C)(C)C=2C=CC(O)=CC=2)C=CC=1C(C)(C)C1=CC=C(O)C=C1 GIXXQTYGFOHYPT-UHFFFAOYSA-N 0.000 description 1
- JZSVLINDCVIUSP-UHFFFAOYSA-N CC(CC(C)C)(C1=CC=C(C=C1)O)C1=CC=C(C=C1)O.C1(CCCCC1)(C1=CC=C(C=C1)O)C1=CC=C(C=C1)O Chemical compound CC(CC(C)C)(C1=CC=C(C=C1)O)C1=CC=C(C=C1)O.C1(CCCCC1)(C1=CC=C(C=C1)O)C1=CC=C(C=C1)O JZSVLINDCVIUSP-UHFFFAOYSA-N 0.000 description 1
- DGERJUKLZWVDQN-UHFFFAOYSA-N CCCCCCCCCCCCCCP.CCCCCCCCCCCCOS(C1=CC=CC=C1)(=O)=O Chemical compound CCCCCCCCCCCCCCP.CCCCCCCCCCCCOS(C1=CC=CC=C1)(=O)=O DGERJUKLZWVDQN-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 102100024693 Death effector domain-containing protein Human genes 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- 101000830359 Homo sapiens Death effector domain-containing protein Proteins 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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- DXIBCWGFAPSVRU-UHFFFAOYSA-N [2-(2-chlorophenyl)phenyl] hydrogen carbonate Chemical compound OC(=O)OC1=CC=CC=C1C1=CC=CC=C1Cl DXIBCWGFAPSVRU-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229920003232 aliphatic polyester Chemical group 0.000 description 1
- 150000001339 alkali metal compounds Chemical class 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 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
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical class ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 description 1
- VBICKXHEKHSIBG-UHFFFAOYSA-N beta-monoglyceryl stearate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- VCCBEIPGXKNHFW-UHFFFAOYSA-N biphenyl-4,4'-diol Chemical group C1=CC(O)=CC=C1C1=CC=C(O)C=C1 VCCBEIPGXKNHFW-UHFFFAOYSA-N 0.000 description 1
- LUQQDEDMRRRWGN-UHFFFAOYSA-N bis(2-bromophenyl) carbonate Chemical compound BrC1=CC=CC=C1OC(=O)OC1=CC=CC=C1Br LUQQDEDMRRRWGN-UHFFFAOYSA-N 0.000 description 1
- DQPSUGZZTADITQ-UHFFFAOYSA-N bis(2-nitrophenyl) carbonate Chemical compound [O-][N+](=O)C1=CC=CC=C1OC(=O)OC1=CC=CC=C1[N+]([O-])=O DQPSUGZZTADITQ-UHFFFAOYSA-N 0.000 description 1
- LGXDMAUHWFVPKO-UHFFFAOYSA-N bis(2-phenylphenyl) carbonate Chemical compound C=1C=CC=C(C=2C=CC=CC=2)C=1OC(=O)OC1=CC=CC=C1C1=CC=CC=C1 LGXDMAUHWFVPKO-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- DEFZNQKDYOBMGU-UHFFFAOYSA-N decyl 2-hydroxybenzoate Chemical compound CCCCCCCCCCOC(=O)C1=CC=CC=C1O DEFZNQKDYOBMGU-UHFFFAOYSA-N 0.000 description 1
- 238000004807 desolvation Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- QLVWOKQMDLQXNN-UHFFFAOYSA-N dibutyl carbonate Chemical compound CCCCOC(=O)OCCCC QLVWOKQMDLQXNN-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- ZOMIMPCSKRRCJI-UHFFFAOYSA-N docosyl 2-hydroxybenzoate Chemical compound CCCCCCCCCCCCCCCCCCCCCCOC(=O)C1=CC=CC=C1O ZOMIMPCSKRRCJI-UHFFFAOYSA-N 0.000 description 1
- CJYBKFFVXWWBMY-UHFFFAOYSA-N dodecyl 2-hydroxybenzoate Chemical compound CCCCCCCCCCCCOC(=O)C1=CC=CC=C1O CJYBKFFVXWWBMY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- TWNBPYIMMRIFEF-UHFFFAOYSA-N ethyl 2-(2-carboxyoxyphenyl)benzoate Chemical compound CCOC(=O)C1=CC=CC=C1C1=CC=CC=C1OC(O)=O TWNBPYIMMRIFEF-UHFFFAOYSA-N 0.000 description 1
- ZQKQZBGDCHBTMC-UHFFFAOYSA-N ethyl 3-carboxyoxy-2-phenylbenzoate Chemical compound CCOC(=O)C1=CC=CC(OC(O)=O)=C1C1=CC=CC=C1 ZQKQZBGDCHBTMC-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 150000002291 germanium compounds Chemical class 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- NHLHASWXBVULGU-UHFFFAOYSA-N hexadecyl 2-hydroxybenzoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C1=CC=CC=C1O NHLHASWXBVULGU-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- OMUKHBXIWYKOGL-UHFFFAOYSA-N methyl 3-carboxyoxy-2-phenylbenzoate Chemical compound COC(=O)C1=CC=CC(OC(O)=O)=C1C1=CC=CC=C1 OMUKHBXIWYKOGL-UHFFFAOYSA-N 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N o-biphenylenemethane Natural products C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 1
- 150000002908 osmium compounds Chemical class 0.000 description 1
- QBDSZLJBMIMQRS-UHFFFAOYSA-N p-Cumylphenol Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=CC=C1 QBDSZLJBMIMQRS-UHFFFAOYSA-N 0.000 description 1
- NKTOLZVEWDHZMU-UHFFFAOYSA-N p-cumyl phenol Natural products CC1=CC=C(C)C(O)=C1 NKTOLZVEWDHZMU-UHFFFAOYSA-N 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 150000004023 quaternary phosphonium compounds Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 description 1
- IFYFNVDTVZKNBZ-UHFFFAOYSA-N tetradecyl 2-hydroxybenzoate Chemical compound CCCCCCCCCCCCCCOC(=O)C1=CC=CC=C1O IFYFNVDTVZKNBZ-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
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 229920006352 transparent thermoplastic Polymers 0.000 description 1
- HTCCWYQPPPBLQT-UHFFFAOYSA-N triacontyl 2-hydroxybenzoate Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCOC(=O)C1=CC=CC=C1O HTCCWYQPPPBLQT-UHFFFAOYSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004260 weight control Methods 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Landscapes
- Polyesters Or Polycarbonates (AREA)
- Optical Record Carriers And Manufacture Thereof (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、成形性を改善した
ポリカーボネート樹脂に関する。さらに詳しくは、ポリ
カーボネート樹脂を成形してなる光記録媒体、とりわけ
高密度記録媒体に関して、スタンパー形状に対する精密
転写性、ハイサイクル成形性に好適であり、且つ、スタ
ンパーへの付着物を極めて抑制した高精密転写性ポリカ
ーボネート樹脂光学用成形材料およびそれより形成され
た光ディスク基板に関する。The present invention relates to a polycarbonate resin having improved moldability. More specifically, with respect to an optical recording medium formed by molding a polycarbonate resin, particularly a high-density recording medium, it is suitable for precision transferability to a stamper shape, high cycle moldability, and extremely low adhesion to the stamper. The present invention relates to a precision transferable polycarbonate resin optical molding material and an optical disk substrate formed therefrom.
【０００２】[0002]
【従来の技術】従来、ポリカーボネート樹脂は、透明
性、耐熱性、機械的特性、寸法安定性が優れていること
から、エンジニアリングプラスチックとして多くの分野
に広く使用されている。特に透明性に優れることから光
学材料、なかでも光ディスクの材料として好適に使用さ
れている。しかし、近年、光ディスクは、高記録密度、
薄肉化が急激に進行しており、またその成形においても
高速サイクル化されておりそのため成形性、なかでも転
写精度について充分ではなかった。そこで、転写精度を
向上させるため、成形機のシリンダー温度を３８０℃程
度、金型温度を１２０℃程度まで高くする必要があっ
た。2. Description of the Related Art Conventionally, polycarbonate resins have been widely used in many fields as engineering plastics because of their excellent transparency, heat resistance, mechanical properties and dimensional stability. Particularly, since it is excellent in transparency, it is suitably used as an optical material, especially as a material for an optical disk. However, in recent years, optical discs have a high recording density,
The thinning has progressed rapidly, and the molding has been cycled at a high speed. Therefore, the moldability, especially the transfer accuracy, has been insufficient. Therefore, in order to improve the transfer accuracy, it is necessary to increase the cylinder temperature of the molding machine to about 380 ° C. and the mold temperature to about 120 ° C.
【０００３】しかしながら、成形温度を高くし、かつ成
形サイクルを高速化すると金型から取り出す際、離型不
良が生じ、ピットやグルーブの形状が変形し、転写精度
が低下するという問題が発生する。However, when the molding temperature is increased and the molding cycle is accelerated, there arises a problem that, when the mold is removed from the mold, mold release failure occurs, the pits and grooves are deformed, and the transfer accuracy is reduced.
【０００４】また、高流動性を付与するために低分子量
体を多く含有する方法が提案されている（特開平９−２
０８６８４号公報、特開平１１−１５５１号公報）。し
かし、この低分子量体は一般に熱安定性が非常に低く、
したがって、成形時に熱分解を促進する結果、ディスク
基板の機械的強度が著しく低下するのみならず、スタン
パーへの付着量が増大する可能性がある。[0004] In addition, a method containing a large amount of low molecular weight substances to impart high fluidity has been proposed (Japanese Patent Laid-Open No. 9-2).
No. 08684, JP-A-11-1551). However, this low molecular weight product generally has very low thermal stability,
Therefore, as a result of promoting thermal decomposition during molding, not only the mechanical strength of the disk substrate is significantly reduced, but also the amount of adhesion to the stamper may increase.
【０００５】[0005]
【発明が解決しようとする課題】本発明の目的は、光記
録媒体、とりわけ高密度記録媒体の製造に関して、スタ
ンパー形状に対する精密転写性、ハイサイクル成形性に
好適であり、且つ、スタンパーへの付着物を極めて抑制
したポリカーボネート樹脂を提供することにある。ここ
で、本発明における「高精密転写性」とは、透明熱可塑
性樹脂成形材料を用いて射出成形により光ディスク基板
を製造する場合に、スタンパーに刻印された微細な凹凸
形状を通常の成形条件で忠実に転写することができる性
質のことを意味する。SUMMARY OF THE INVENTION It is an object of the present invention to manufacture an optical recording medium, especially a high-density recording medium, which is suitable for precision transferability to a stamper shape and high cycle molding property, and for attaching to a stamper. An object of the present invention is to provide a polycarbonate resin in which kimono is extremely suppressed. Here, “high precision transferability” in the present invention means that when an optical disc substrate is manufactured by injection molding using a transparent thermoplastic resin molding material, the fine irregularities stamped on the stamper are formed under normal molding conditions. It means the property that can be faithfully transferred.
【０００６】本発明者らは、上記目的を達成せんと鋭意
研究を重ねた結果、ポリカーボネート樹脂において、流
動特性、粘弾性特性、機械特性を主として支配している
高分子量体および低分子量体の含有量を特定量に規定す
ることにより、スタンパー形状に対する精密転写性、ハ
イサイクル成形性に好適であり、且つ、スタンパーへの
付着物を極めて抑制したポリカーボネート樹脂が得られ
ることを見出した。本発明はこの知見に基づき完成した
ものである。The inventors of the present invention have conducted intensive studies to achieve the above object. As a result, the polycarbonate resin contained a high molecular weight substance and a low molecular weight substance which mainly governed the flow properties, viscoelastic properties and mechanical properties. By defining the amount to be a specific amount, it has been found that a polycarbonate resin which is suitable for precision transferability to a stamper shape and high cycle moldability and in which adhesion to the stamper is extremely suppressed can be obtained. The present invention has been completed based on this finding.
【０００７】[0007]
【課題を解決するための手段】すなわち、本発明におい
ては、ポリカーボネート樹脂において、流動特性、粘弾
性特性、機械特性を主として支配している高分子量体に
ついては６０,０００以上の分子量成分、また低分子量
体については１０,０００以下の２クラスに着目した。
そのうち６０,０００以上の高分子量ポリカーボネート
樹脂は、全重量組成中の１２重量％以下であり、また１
０,０００以下の低分子量ポリカーボネート樹脂が、全
重量組成中の９〜２６重量％の範囲であることを特徴と
するポリカーボネート樹脂が提供される。That is, according to the present invention, in the polycarbonate resin, a high molecular weight component mainly controlling flow properties, viscoelastic properties and mechanical properties of a polycarbonate resin has a molecular weight component of 60,000 or more and a low molecular weight component. As for the molecular weight, attention was focused on two classes of 10,000 or less.
Among them, 60,000 or more of high molecular weight polycarbonate resin accounts for 12% by weight or less of the total weight composition, and
A polycarbonate resin is provided, wherein the low molecular weight polycarbonate resin having a molecular weight of not more than 000 is in the range of 9 to 26% by weight of the total weight composition.
【０００８】本発明においては、６０,０００以上の高
分子量ポリカーボネート樹脂成分が、全重量組成中の１
２重量％以下、好ましくは１０重量％以下、より好まし
くは８重量％以下であり、また１０,０００以下の低分
子量ポリカーボネート樹脂成分が、全重量組成中の９〜
２６重量％、好ましくは９〜２０重量％、より好ましく
は９〜１７重量％の範囲である芳香族ポリカーボネート
樹脂を提供することによって、ディスク成形に際して、
高密度ディスクに対するより精密な転写性とスタンパー
への付着物の低減について、ディスク強度を損ねること
なく、成形可能となる。In the present invention, 60,000 or more high molecular weight polycarbonate resin components are contained in the total weight composition.
2% by weight or less, preferably 10% by weight or less, more preferably 8% by weight or less, and 10,000 or less of a low-molecular-weight polycarbonate resin component accounts for 9 to 9% of the total weight composition.
By providing an aromatic polycarbonate resin in the range of 26% by weight, preferably 9-20% by weight, more preferably 9-17% by weight, during disc molding,
With respect to more precise transferability to a high-density disc and reduction of deposits on a stamper, molding can be performed without impairing disc strength.
【０００９】かかるポリカーボネート樹脂としては、以
下説明するものが使用される。すなわち、ポリカーボネ
ート樹脂は、通常二価フェノールとカーボネート前駆体
とを界面重合法（溶液法）または溶融重合法で反応させ
て得られるものである。ここで使用される二価フェノー
ルの代表的な例としては、ハイドロキノン、レゾルシノ
ール、４,４’−ジヒドロキシジフェニル、ビス（４−
ヒドロキシフェニル）メタン、ビス｛（４−ヒドロキシ
−３,５−ジメチル）フェニル｝メタン、１,１−ビス
（４−ヒドロキシフェニル）エタン、１,１−ビス（４
−ヒドロキシフェニル）−１−フェニルエタン、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）、２,２−ビス｛（４−ヒドロキシ−３
−メチル）フェニル｝プロパン、２,２−ビス｛（４−
ヒドロキシ−３,５−ジメチル）フェニル｝プロパン、
２,２−ビス｛（３,５−ジブロモ−４−ヒドロキシ）フ
ェニル｝プロパン、２,２−ビス｛（３−イソプロピル
−４−ヒドロキシ）フェニル｝プロパン、２,２−ビス
｛（４−ヒドロキシ−３−フェニル）フェニル｝プロパ
ン、２,２−ビス（４−ヒドロキシフェニル）ブタン、
２,２−ビス（４−ヒドロキシフェニル）−３−メチル
ブタン、２,２−ビス（４−ヒドロキシフェニル）−３,
３−ジメチルブタン、２,４−ビス（４−ヒドロキシフ
ェニル）−２−メチルブタン、２,２−ビス（４−ヒド
ロキシフェニル）ペンタン、２,２−ビス（４−ヒドロ
キシフェニル）−４−メチルペンタン、１,１−ビス
（４−ヒドロキシフェニル）シクロヘキサン、１,１−
ビス（４−ヒドロキシフェニル）−４−イソプロピルシ
クロヘキサン、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、９,９−
ビス（４−ヒドロキシフェニル）フルオレン、９,９−
ビス｛（４−ヒドロキシ−３−メチル）フェニル｝フル
オレン、α,α’−ビス（４−ヒドロキシフェニル）−
ｏ−ジイソプロピルベンゼン、α,α’−ビス（４−ヒ
ドロキシフェニル）−ｍ−ジイソプロピルベンゼン、
α,α’−ビス（４−ヒドロキシフェニル）−ｐ−ジイ
ソプロピルベンゼン、１,３−ビス（４−ヒドロキシフ
ェニル）−５,７−ジメチルアダマンタン、４,４’−ジ
ヒドロキシジフェニルスルホン、４,４’−ジヒドロキ
シジフェニルスルホキシド、４,４’−ジヒドロキシジ
フェニルスルフィド、４,４’−ジヒドロキシジフェニ
ルケトン、４,４’−ジヒドロキシジフェニルエーテル
および４,４’−ジヒドロキシジフェニルエステル等が
挙げられ、これらは単独または２種以上を混合して使用
できる。As the polycarbonate resin, those described below are used. That is, the polycarbonate resin is usually obtained by reacting a dihydric phenol with a carbonate precursor by an interfacial polymerization method (solution method) or a melt polymerization method. Representative examples of the dihydric phenol used herein include hydroquinone, resorcinol, 4,4'-dihydroxydiphenyl, bis (4-
Hydroxyphenyl) methane, bis {(4-hydroxy-3,5-dimethyl) phenyl} methane, 1,1-bis (4-hydroxyphenyl) ethane, 1,1-bis (4
-Hydroxyphenyl) -1-phenylethane, 2,2
-Bis (4-hydroxyphenyl) propane (commonly known as bisphenol A), 2,2-bis} (4-hydroxy-3
-Methyl) phenyl {propane, 2,2-bis} (4-
(Hydroxy-3,5-dimethyl) phenyl} propane,
2,2-bis {(3,5-dibromo-4-hydroxy) phenyl} propane, 2,2-bis {(3-isopropyl-4-hydroxy) phenyl} propane, 2,2-bis} (4-hydroxy -3-phenyl) phenyl} propane, 2,2-bis (4-hydroxyphenyl) butane,
2,2-bis (4-hydroxyphenyl) -3-methylbutane, 2,2-bis (4-hydroxyphenyl) -3,
3-dimethylbutane, 2,4-bis (4-hydroxyphenyl) -2-methylbutane, 2,2-bis (4-hydroxyphenyl) pentane, 2,2-bis (4-hydroxyphenyl) -4-methylpentane 1,1-bis (4-hydroxyphenyl) cyclohexane, 1,1-
Bis (4-hydroxyphenyl) -4-isopropylcyclohexane, 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane, 9,9-
Bis (4-hydroxyphenyl) fluorene, 9,9-
Bis {(4-hydroxy-3-methyl) phenyl} fluorene, α, α′-bis (4-hydroxyphenyl)-
o-diisopropylbenzene, α, α′-bis (4-hydroxyphenyl) -m-diisopropylbenzene,
α, α′-bis (4-hydroxyphenyl) -p-diisopropylbenzene, 1,3-bis (4-hydroxyphenyl) -5,7-dimethyladamantane, 4,4′-dihydroxydiphenylsulfone, 4,4 ′ -Dihydroxydiphenyl sulphoxide, 4,4'-dihydroxydiphenyl sulfide, 4,4'-dihydroxydiphenyl ketone, 4,4'-dihydroxydiphenyl ether and 4,4'-dihydroxydiphenyl ester; These can be used in combination.
【００１０】なかでもビスフェノールＡ、２,２−ビス
｛（４−ヒドロキシ−３−メチル）フェニル｝プロパ
ン、２,２−ビス（４−ヒドロキシフェニル）ブタン、
２,２−ビス（４−ヒドロキシフェニル）−３−メチル
ブタン、２,２−ビス（４−ヒドロキシフェニル）−３,
３−ジメチルブタン、２,２−ビス（４−ヒドロキシフ
ェニル）−４−メチルペンタン、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
サンおよびα,α’−ビス（４−ヒドロキシフェニル）
−ｍ−ジイソプロピルベンゼンからなる群より選ばれた
少くとも１種のビスフェノールより得られる単独重合体
または共重合体が好ましく、特に、ビスフェノールＡの
単独重合体および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とビスフェ
ノールＡ、２,２−ビス｛（４−ヒドロキシ−３−メチ
ル）フェニル｝プロパンまたはα,α’−ビス（４−ヒ
ドロキシフェニル）−ｍ−ジイソプロピルベンゼンとの
共重合体が好ましく使用される。Among them, bisphenol A, 2,2-bis {(4-hydroxy-3-methyl) phenyl} propane, 2,2-bis (4-hydroxyphenyl) butane,
2,2-bis (4-hydroxyphenyl) -3-methylbutane, 2,2-bis (4-hydroxyphenyl) -3,
3-dimethylbutane, 2,2-bis (4-hydroxyphenyl) -4-methylpentane, 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane and α, α′-bis ( 4-hydroxyphenyl)
Homopolymers or copolymers obtained from at least one bisphenol selected from the group consisting of -m-diisopropylbenzene are preferred, and in particular, a homopolymer of bisphenol A and 1,1-bis (4-hydroxyphenyl) ) -3,3,5-Trimethylcyclohexane and bisphenol A, 2,2-bis {(4-hydroxy-3-methyl) phenyl} propane or α, α′-bis (4-hydroxyphenyl) -m-diisopropylbenzene Is preferably used.
【００１１】カーボネート前駆体としてはカルボニルハ
ライド、カーボネートエステルまたはハロホルメート等
が使用され、具体的にはホスゲン、ジフェニルカーボネ
ートまたは二価フェノールのジハロホルメート等が挙げ
られる。As the carbonate precursor, carbonyl halide, carbonate ester or haloformate is used, and specific examples include phosgene, diphenyl carbonate, dihaloformate of dihydric phenol and the like.
【００１２】上記二価フェノールとカーボネート前駆体
を界面重合法（溶液法）または溶融重合法によって反応
させてポリカーボネート樹脂を製造するに当っては、必
要に応じて触媒、末端停止剤、二価フェノールの酸化防
止剤等を使用してもよい。またポリカーボネート樹脂は
三官能以上の多官能性芳香族化合物を共重合した分岐ポ
リカーボネート樹脂であっても、芳香族または脂肪族の
二官能性カルボン酸を共重合したポリエステルカーボネ
ート樹脂であってもよく、また、得られたポリカーボネ
ート樹脂の２種以上を混合した混合物であってもよい。In producing the polycarbonate resin by reacting the dihydric phenol with the carbonate precursor by an interfacial polymerization method (solution method) or a melt polymerization method, if necessary, a catalyst, a terminal stopper, a dihydric phenol, May be used. Further, the polycarbonate resin may be a branched polycarbonate resin obtained by copolymerizing a trifunctional or higher polyfunctional aromatic compound, or a polyester carbonate resin obtained by copolymerizing an aromatic or aliphatic bifunctional carboxylic acid, Further, a mixture of two or more of the obtained polycarbonate resins may be used.
【００１３】界面重合法（溶液法）による反応は、通常
二価フェノールとホスゲンとの反応であり、酸結合剤お
よび有機溶媒の存在下に反応させる。酸結合剤として
は、例えば水酸化ナトリウム、水酸化カリウム等のアル
カリ金属水酸化物またはピリジン等のアミン化合物が用
いられる。有機溶媒としては、例えば塩化メチレン、ク
ロロベンゼン等のハロゲン化炭化水素が用いられる。ま
た、反応促進のために例えばトリエチルアミン、テトラ
−ｎ−ブチルアンモニウムブロマイド、テトラ−ｎ−ブ
チルホスホニウムブロマイド等の第三級アミン、第四級
アンモニウム化合物、第四級ホスホニウム化合物等の触
媒を用いることもできる。その際、反応温度は通常０〜
４０℃、反応時間は１０分〜５時間程度、反応中のｐＨ
は９以上に保つのが好ましい。The reaction by the interfacial polymerization method (solution method) is usually a reaction between dihydric phenol and phosgene, and is carried out in the presence of an acid binder and an organic solvent. As the acid binder, for example, an alkali metal hydroxide such as sodium hydroxide or potassium hydroxide or an amine compound such as pyridine is used. As the organic solvent, for example, halogenated hydrocarbons such as methylene chloride and chlorobenzene are used. Further, for promoting the reaction, for example, a catalyst such as a tertiary amine such as triethylamine, tetra-n-butylammonium bromide, or tetra-n-butylphosphonium bromide, a quaternary ammonium compound, or a quaternary phosphonium compound may be used. it can. At that time, the reaction temperature is usually 0 to
40 ° C., reaction time is about 10 minutes to 5 hours, pH during the reaction
Is preferably maintained at 9 or more.
【００１４】また、かかる重合反応において、通常末端
停止剤が使用される。かかる末端停止剤として単官能フ
ェノール類を使用することができる。単官能フェノール
類は末端停止剤として分子量調節のために一般的に使用
され、また得られたポリカーボネート樹脂は、末端が単
官能フェノール類に基づく基によって封鎖されているの
で、そうでないものと比べて熱安定性に優れている。か
かる単官能フェノール類としては、一般にはフェノール
または低級アルキル置換フェノールであって、下記一般
式で表される単官能フェノール類を示すことができる。In such a polymerization reaction, a terminal stopper is usually used. Monofunctional phenols can be used as such a terminal stopper. Monofunctional phenols are commonly used as molecular terminators for molecular weight control, and the resulting polycarbonate resins are capped by groups based on monofunctional phenols, so that Excellent heat stability. Such a monofunctional phenol is generally a phenol or a lower alkyl-substituted phenol, and may be a monofunctional phenol represented by the following general formula.
【００１５】[0015]
【化１】 Embedded image
【００１６】［式中、Ａは水素原子または炭素数１〜９
の直鎖または分岐のアルキル基あるいはフェニル置換ア
ルキル基であり、ｒは１〜５、好ましくは１〜３の整数
である。］ 上記単官能フェノール類の具体例としては、例えばフェ
ノール、ｐ−ｔｅｒｔ−ブチルフェノール、ｐ−クミル
フェノールおよびイソオクチルフェノールが挙げられ
る。Wherein A is a hydrogen atom or a carbon number of 1 to 9
Is a linear or branched alkyl group or a phenyl-substituted alkyl group, and r is an integer of 1 to 5, preferably 1 to 3. Specific examples of the monofunctional phenols include phenol, p-tert-butylphenol, p-cumylphenol, and isooctylphenol.
【００１７】また、他の単官能フェノール類としては、
長鎖のアルキル基あるいは脂肪族ポリエステル基を置換
基として有するフェノール類または安息香酸クロライド
類、もしくは長鎖のアルキルカルボン酸クロライド類を
使用することができ、これらを用いてポリカーボネート
共重合体の末端を封鎖すると、これらは末端停止剤また
は分子量調節剤として機能するのみならず、樹脂の溶融
流動性が改良され、成形加工が容易になるばかりでな
く、基板としての物性、特に樹脂の吸水率を低くする効
果があり、また基板の複屈折率が低減される効果もあ
り、好ましく使用される。なかでも、下記一般式（２）
および（３）で表される長鎖のアルキル基を置換基とし
て有するフェノール類が好ましく使用される。Further, other monofunctional phenols include:
Phenols or benzoic acid chlorides having a long-chain alkyl group or an aliphatic polyester group as a substituent, or long-chain alkyl carboxylic acid chlorides can be used. When blocked, these not only function as a terminal terminator or a molecular weight regulator, but also improve the melt flowability of the resin, not only facilitate the molding process, but also reduce the physical properties as a substrate, especially the water absorption of the resin. It has the effect of reducing the birefringence of the substrate, and is preferably used. Above all, the following general formula (2)
Phenols having a long-chain alkyl group represented by and (3) as a substituent are preferably used.
【００１８】[0018]
【化２】 Embedded image
【００１９】[0019]
【化３】 Embedded image
【００２０】［式中、Ｘは−Ｒ−Ｏ−、−Ｒ−ＣＯ−Ｏ
−または−Ｒ−Ｏ−ＣＯ−である、ここでＲは単結合ま
たは炭素数１〜１０、好ましくは１〜５の二価の脂肪族
炭化水素基を示し、ｎは１０〜５０の整数を示す。］ 前記式（２）の置換フェノール類としてはｎが１０〜３
０、特に１０〜２６のものが好ましく、その具体例とし
ては例えばデシルフェノール、ドデシルフェノール、テ
トラデシルフェノール、ヘキサデシルフェノール、オク
タデシルフェノール、エイコシルフェノール、ドコシル
フェノールおよびトリアコンチルフェノール等を挙げる
ことができる。Wherein X is -RO-, -R-CO-O
— Or —RO—CO—, wherein R represents a single bond or a divalent aliphatic hydrocarbon group having 1 to 10, preferably 1 to 5 carbon atoms, and n represents an integer of 10 to 50. Show. As the substituted phenols of the formula (2), n is 10 to 3
0, and particularly preferably 10 to 26, and specific examples thereof include, for example, decylphenol, dodecylphenol, tetradecylphenol, hexadecylphenol, octadecylphenol, eicosylphenol, docosylphenol, and tricontylphenol. Can be.
【００２１】また、前記式（３）の置換フェノール類と
してはＸが−Ｒ−ＣＯ−Ｏ−であり、Ｒが単結合である
化合物が適当であり、ｎが１０〜３０、特に１０〜２６
のものが好適であって、その具体例としては例えばヒド
ロキシ安息香酸デシル、ヒドロキシ安息香酸ドデシル、
ヒドロキシ安息香酸テトラデシル、ヒドロキシ安息香酸
ヘキサデシル、ヒドロキシ安息香酸エイコシル、ヒドロ
キシ安息香酸ドコシルおよびヒドロキシ安息香酸トリア
コンチルが挙げられる。Further, as the substituted phenols of the formula (3), a compound in which X is -R-CO-O- and R is a single bond is suitable, and n is 10 to 30, especially 10 to 26.
Are preferred, and specific examples thereof include, for example, decyl hydroxybenzoate, dodecyl hydroxybenzoate,
Examples include tetradecyl hydroxybenzoate, hexadecyl hydroxybenzoate, eicosyl hydroxybenzoate, docosyl hydroxybenzoate and triacontyl hydroxybenzoate.
【００２２】これらの末端停止剤は、得られたポリカー
ボネート樹脂の全末端に対して少くとも５モル％、好ま
しくは少くとも１０モル％末端に導入されることが望ま
しく、また、末端停止剤は単独でまたは２種以上混合し
て使用してもよい。It is desirable that these terminal stoppers are introduced at least at 5 mol%, preferably at least 10 mol%, based on all terminals of the obtained polycarbonate resin. Or a mixture of two or more.
【００２３】溶融重合法による反応は、通常二価フェノ
ールとカーボネートエステルとのエステル交換反応であ
り、不活性ガスの存在下に二価フェノールとカーボネー
トエステルとを加熱しながら混合して、生成するアルコ
ールまたはフェノール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の
沸点等により異なるが、通常１２０〜３５０℃の範囲で
ある。反応後期には系を１３３０〜１３.３Ｐａ程度に
減圧して生成するアルコールまたはフェノールの留出を
容易にさせる。反応時間は通常１〜４時間程度である。The reaction by the melt polymerization method is usually a transesterification reaction between a dihydric phenol and a carbonate ester. The dihydric phenol and the carbonate ester are mixed while heating in the presence of an inert gas to form an alcohol. Alternatively, it is carried out by a method of distilling phenol. The reaction temperature varies depending on the boiling point of the produced alcohol or phenol, but is usually in the range of 120 to 350 ° C. In the latter stage of the reaction, the pressure of the system is reduced to about 1330 to 13.3 Pa to facilitate the distillation of alcohol or phenol produced. The reaction time is usually about 1 to 4 hours.
【００２４】カーボネートエステルとしては、置換され
ていてもよい炭素数６〜１０のアリール基、アラルキル
基あるいは炭素数１〜４のアルキル基などのエステルが
挙げられる。具体的にはジフェニルカーボネート、ジト
ルイルカーボネート、ビス（クロロフェニル）カーボネ
ート、ジナフチルカーボネート、ビス（ジフェニル）カ
ーボネート、ジメチルカーボネート、ジエチルカーボネ
ート、ジブチルカーボネートなどが挙げられ、なかでも
ジフェニルカーボネートが好ましい。Examples of the carbonate ester include an optionally substituted ester such as an aryl group having 6 to 10 carbon atoms, an aralkyl group or an alkyl group having 1 to 4 carbon atoms. Specifically, diphenyl carbonate, ditolyl carbonate, bis (chlorophenyl) carbonate, dinaphthyl carbonate, bis (diphenyl) carbonate, dimethyl carbonate, diethyl carbonate, dibutyl carbonate and the like can be mentioned, among which diphenyl carbonate is preferable.
【００２５】また、重合速度を高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、例えば水
酸化ナトリウム、水酸化カリウム、二価フェノールのナ
トリウム塩、カリウム塩等のアルカリ金属化合物；水酸
化カルシウム、水酸化バリウム、水酸化マグネシウム等
のアルカリ土類金属化合物；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、トリメチルアミン、トリエチルアミン等の含窒素塩
基性化合物；アルカリ金属やアルカリ土類金属のアルコ
キシド類；アルカリ金属やアルカリ土類金属の有機酸塩
類；その他に亜鉛化合物類、ホウ素化合物類、アルミニ
ウム化合物類、珪素化合物類、ゲルマニウム化合物類、
有機スズ化合物類、鉛化合物類、オスミウム化合物類、
アンチモン化合物類マンガン化合物類、チタン化合物
類、ジルコニウム化合物類などの通常エステル化反応、
エステル交換反応に使用される触媒を用いることができ
る。触媒は単独で使用してもよいし、２種以上組み合わ
せ使用してもよい。これらの重合触媒の使用量は、原料
の二価フェノール１モルに対し、好ましくは１×１０-8
〜１×１０-3当量、より好ましくは１×１０-7〜５×１
０-4当量の範囲で選ばれる。In order to increase the polymerization rate, a polymerization catalyst can be used. Examples of the polymerization catalyst include alkali metal compounds such as sodium hydroxide, potassium hydroxide, and sodium and potassium salts of dihydric phenol; Alkaline earth metal compounds such as calcium oxide, barium hydroxide and magnesium hydroxide; nitrogen-containing basic compounds such as tetramethylammonium hydroxide, tetraethylammonium hydroxide, trimethylamine and triethylamine; alkoxides of alkali metals and alkaline earth metals Organic acid salts of alkali metals and alkaline earth metals; zinc compounds, boron compounds, aluminum compounds, silicon compounds, germanium compounds;
Organic tin compounds, lead compounds, osmium compounds,
Normal esterification reaction of antimony compounds manganese compounds, titanium compounds, zirconium compounds, etc.
The catalyst used for the transesterification can be used. The catalyst may be used alone or in combination of two or more. The amount of the polymerization catalyst used is preferably 1 × 10 −8 to 1 mol of the starting dihydric phenol.
１1 × 10 −3 equivalents, more preferably 1 × 10 −7 to 5 × 1
It is selected in the range of 0-4 equivalents.
【００２６】また、かかる重合反応において、フェノー
ル性の末端基を減少するために、重縮反応の後期あるい
は終了後に、例えばビス（クロロフェニル）カーボネー
ト、ビス（ブロモフェニル）カーボネート、ビス（ニト
ロフェニル）カーボネート、ビス（フェニルフェニル）
カーボネート、クロロフェニルフェニルカーボネート、
ブロモフェニルフェニルカーボネート、ニトロフェニル
フェニルカーボネート、フェニルフェニルカーボネー
ト、メトキシカルボニルフェニルフェニルカーボネート
およびエトキシカルボニルフェニルフェニルカーボネー
ト等の化合物を加えることが好ましい。なかでも２−ク
ロロフェニルフェニルカーボネート、２−メトキシカル
ボニルフェニルフェニルカーボネートおよび２−エトキ
シカルボニルフェニルフェニルカーボネートが好まし
く、特に２−メトキシカルボニルフェニルフェニルカー
ボネートが好ましく使用される。In the polymerization reaction, in order to reduce the number of phenolic terminal groups, for example, bis (chlorophenyl) carbonate, bis (bromophenyl) carbonate, bis (nitrophenyl) carbonate is used later or after completion of the polycondensation reaction. , Bis (phenylphenyl)
Carbonate, chlorophenylphenyl carbonate,
It is preferable to add compounds such as bromophenylphenyl carbonate, nitrophenylphenyl carbonate, phenylphenyl carbonate, methoxycarbonylphenylphenyl carbonate, and ethoxycarbonylphenylphenyl carbonate. Of these, 2-chlorophenylphenyl carbonate, 2-methoxycarbonylphenylphenyl carbonate and 2-ethoxycarbonylphenylphenyl carbonate are preferred, and 2-methoxycarbonylphenylphenyl carbonate is particularly preferred.
【００２７】本発明では、かくして得られた芳香族ポリ
カーボネート樹脂の分子量が、ゲルパーミエーションク
ロマトグラフィー（ＧＰＣ）で測定する重量平均分子量
が２４,０００〜４０,０００の範囲に制御されたものを
使用する。この重量平均分子量が、２４,０００未満で
は基板としての強度に問題があり、また４０,０００を
越えると成形時の溶融流動性が悪く、基板に好ましくな
い光学歪みが増大する。上記の観点からポリカーボネー
ト樹脂の分子量は、重量平均分子量（Ｍｗ）で２６,０
００〜４０,０００が好ましく、２６,０００〜３６,０
００がより好ましく、２７,５００〜３３,０００が特に
好ましい。かかる重量平均分子量を有するポリカーボネ
ート樹脂は、光学用材料として十分な強度が得られ、ま
た、成形時の溶融流動性も良好であり成形歪みが発生せ
ず好ましい。In the present invention, the aromatic polycarbonate resin thus obtained has a molecular weight controlled by gel permeation chromatography (GPC) within a range of 24,000 to 40,000. I do. If the weight average molecular weight is less than 24,000, there is a problem in the strength as a substrate. If it exceeds 40,000, the melt fluidity during molding is poor, and undesired optical distortion of the substrate increases. From the above viewpoint, the molecular weight of the polycarbonate resin is 26.0, in terms of weight average molecular weight (Mw).
00 to 40,000 is preferable, and 26,000 to 36.0.
00 is more preferable, and 27,500 to 33,000 is particularly preferable. A polycarbonate resin having such a weight average molecular weight is preferable because sufficient strength can be obtained as an optical material, and the melt fluidity during molding is good and molding distortion does not occur.
【００２８】本発明では、芳香族ポリカーボネート樹脂
の重量平均分子量が、上記範囲内にあるのと同時に、該
樹脂中に含まれる１０,０００以下の分子量成分が９〜
２６重量％の範囲であり、かつ６０,０００以上の分子
量成分が１２重量％以下であることが肝要である。In the present invention, the weight average molecular weight of the aromatic polycarbonate resin is within the above range, and at the same time, the molecular weight component of 10,000 or less contained in the resin is 9 to 10%.
It is important that the content is in the range of 26% by weight and the molecular weight component of 60,000 or more is 12% by weight or less.
【００２９】上述した要件を満足すべく、重量平均分子
量を制御するためには、高分子量成分量、および低分子
量成分量の制御が必要となる。このうち、高分子量成分
量の制御方法としては、（ａ）ポリカーボネートの重縮
合反応において、重量平均分子量を２４,０００程度に
設定して、高分子量成分の生成量を抑制する方法、
（ｂ）界面重合法（溶液法）において、重合が終了した
後のポリカーボネート樹脂溶液にアセトン、ＭＥＫなど
の高分子量ポリカーボネートに対する貧溶媒を添加せし
め、析出初期における高分子量ポリカーボネート樹脂を
多く含む析出物を濾過し、残りの溶液を乾燥・固化して
高分子量成分を除去する方法、（ｃ）適度な良溶媒性を
示す溶媒、例えば塩化メチレン／アセトン、塩化メチレ
ン／ｎ−ヘプタン、ジオキソラン／ＭＥＫ、ジオキソラ
ン／アセトンの混合溶媒等を用いて、ポリカーボネート
樹脂の大部分（６０〜９８重量％、好ましくは７０〜９
５重量％）を溶解し、この溶液を乾燥・固化して中分子
量成分を多く含ませる方法、（ｄ）ゲルパーミエーショ
ンクロマトグラフィー法（ＧＰＣ法）を使用して、分画
分取をおこなうことにより、高分子量のポリカーボネー
トを除去する方法などが挙げられるが、特に限定される
ものではない。In order to control the weight average molecular weight so as to satisfy the above requirements, it is necessary to control the amount of high molecular weight components and the amount of low molecular weight components. Among these, as the method of controlling the amount of the high molecular weight component, (a) a method of setting the weight average molecular weight to about 24,000 in the polycondensation reaction of the polycarbonate to suppress the generation amount of the high molecular weight component,
(B) In the interfacial polymerization method (solution method), a poor solvent for a high molecular weight polycarbonate such as acetone or MEK is added to the polycarbonate resin solution after the completion of the polymerization, and a precipitate containing a large amount of the high molecular weight polycarbonate resin in the initial stage of the precipitation is added. A method of removing the high molecular weight component by filtering and drying and solidifying the remaining solution, (c) a solvent having a moderately good solvent property, for example, methylene chloride / acetone, methylene chloride / n-heptane, dioxolan / MEK, dioxolan Of the polycarbonate resin (60 to 98% by weight, preferably 70 to 9% by weight) using a mixed solvent of
5% by weight), and drying and solidifying the solution to increase the amount of medium molecular weight components. (D) Separation and fractionation using gel permeation chromatography (GPC) For removing high-molecular-weight polycarbonate, but there is no particular limitation.
【００３０】また、低分子量成分量を制御する方法とし
ては、（１）アセトンなどが、高分子量ポリカーボネー
トに対する貧溶媒と同時に比較的低分子量のポリカーボ
ネートに対しては、溶解力があるという特性を有する事
を利用して、加熱条件下で、造粒（脱溶媒）後の粒状原
料をアセトンなどで洗浄することで抽出除去する方法、
（２）界面重合法（溶液法）において、重合が終了した
後のポリカーボネート樹脂溶液にアセトン、ＭＥＫなど
の高分子量ポリカーボネートに対する貧溶媒を添加せし
める。析出発生後、さらに攪拌を継続することにより、
熟成を進行させ、低分子量ポリカーボネート樹脂を該溶
液に溶解させたまま、中分子量以上のポリカーボネート
成分を多く含む析出物を濾取し、これを乾燥・固化して
低分子量成分を除去する方法などが挙げられるが、特に
限定されるものではない。これらの中でも（ａ）〜
（ｄ）の高分子量成分を制御する方法と（１）〜（２）
の低分子量成分を制御する方法を組合わせるた方法が好
ましい。As a method for controlling the amount of the low molecular weight component, (1) acetone or the like has a property that it has a dissolving power for a relatively low molecular weight polycarbonate as well as a poor solvent for a high molecular weight polycarbonate. A method of extracting and removing the granular raw material after granulation (desolvation) by washing with acetone or the like under heating conditions,
(2) In the interfacial polymerization method (solution method), a poor solvent for a high molecular weight polycarbonate such as acetone or MEK is added to the polycarbonate resin solution after the polymerization is completed. After precipitation occurs, by continuing stirring,
Aging is advanced, and while the low-molecular-weight polycarbonate resin is dissolved in the solution, a precipitate containing a large amount of a medium-molecular-weight or more polycarbonate component is collected by filtration, and dried and solidified to remove the low-molecular-weight component. Although it is mentioned, it is not particularly limited. Among these, (a) ~
Method (d) for controlling the high molecular weight component and (1) to (2)
Is preferred in combination with the method for controlling low molecular weight components of the above.
【００３１】原料ポリカーボネート樹脂は、従来公知の
常法（界面重合法（溶液法）、溶融重合法など）により
製造した後、溶液状態において濾過処理を行ない未反応
成分等の不純物や異物を除去することが好ましい。更に
射出成形に供するためのペレット状ポリカーボネート樹
脂を得る押出工程（ペレット化工程）では溶融状態の時
に濾過精度１０μｍの焼結金属フィルターを通すなどし
て異物を除去したりすることが好ましい。必要により、
例えばリン系等の酸化防止剤などの添加剤を加えること
も好ましい。いずれにしても射出成形前の原料樹脂は異
物、不純物、溶媒などの含有量を極力低くしておくこと
が必要である。The raw material polycarbonate resin is produced by a conventionally known method (interfacial polymerization method (solution method), melt polymerization method, etc.) and then filtered in a solution state to remove impurities and foreign substances such as unreacted components. Is preferred. Further, in the extrusion step (pelletizing step) of obtaining a pellet-like polycarbonate resin for use in injection molding, it is preferable to remove foreign matter by passing through a sintered metal filter having a filtration accuracy of 10 μm in a molten state. If necessary,
For example, it is also preferable to add an additive such as a phosphorus-based antioxidant. In any case, it is necessary to minimize the content of foreign materials, impurities, solvents and the like in the raw material resin before injection molding.
【００３２】上記ポリカーボネート樹脂より光ディスク
基板を製造する場合には射出成形機（射出圧縮成形機を
含む）を用いる。この射出成形機としては一般的に使用
されているものでよいが、炭化物の発生を抑制しディス
ク基板の信頼性を高める観点からシリンダーやスクリュ
ーとして樹脂との付着性が低く、かつ耐食性、耐摩耗性
を示す材料を使用してなるものを用いるのが好ましい。
射出成形の条件としてはシリンダー温度３００〜４００
℃、金型温度５０〜１４０℃が好ましく、これらにより
光学的に優れた光ディスク基板を得ることができる。成
形工程での環境は、本発明の目的から考えて、可能な限
りクリーンであることが好ましい。また、成形に供する
材料を十分乾燥して水分を除去することや、溶融樹脂の
分解を招くような滞留を起こさないように配慮すること
も重要となる。When an optical disk substrate is manufactured from the above polycarbonate resin, an injection molding machine (including an injection compression molding machine) is used. As this injection molding machine, a commonly used one may be used, but from the viewpoint of suppressing the generation of carbides and increasing the reliability of the disk substrate, the adhesion to the resin as a cylinder or a screw is low, and the corrosion resistance and abrasion resistance are low. It is preferable to use a material made of a material having properties.
Injection molding conditions are cylinder temperature 300-400.
C. and a mold temperature of 50 to 140 ° C. are preferred, whereby an optically excellent optical disc substrate can be obtained. The environment in the molding step is preferably as clean as possible from the viewpoint of the present invention. It is also important to sufficiently dry the material to be subjected to molding to remove moisture, and to take care not to cause stagnation that may cause decomposition of the molten resin.
【００３３】このように成形された光ディスク基板は、
コンパクトディスク（以下、ＣＤと称することがあ
る）、ＣＤ−Ｒ、ＭＯ、ＭＤ−ＭＯ等や、更にはデジタ
ルビデオディスク（以下、ＤＶＤと称することがあ
る）、ＤＶＤ−ＲＯＭ、ＤＶＤ−ａｕｄｉｏ、ＤＶＤ−
Ｒ、ＤＶＤ−ＲＡＭ等で代表される高密度光ディスク用
基板として、使用される。特に高密度ディスクに好適に
用いられる。The optical disk substrate thus formed is:
Compact disc (hereinafter, sometimes referred to as CD), CD-R, MO, MD-MO, etc., and further, digital video disc (hereinafter, sometimes referred to as DVD), DVD-ROM, DVD-audio, DVD −
It is used as a substrate for high-density optical disks represented by R, DVD-RAM, and the like. Particularly, it is suitably used for a high-density disk.
【００３４】[0034]
【実施例】以下、実施例を挙げて詳細に説明するが、本
発明は何らこれに限定されるものではない。なお評価は
下記の方法に従った。The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples. The evaluation was performed according to the following method.
【００３５】（１）重量平均分子量および分子量分布 ゲルパーミエーションクロマトグラフィー法（ＧＰＣ
法）によるポリスチレン換算測定を実施した。すなわ
ち、ＧＰＣ充填剤としては、Ｓｈｏｄｅｘ ＧＰＣＡ−
８０４を充填した内径１.５ｃｍ、長さ４６ｃｍのカラ
ムを使用する。まず、以下の標準ポリスチレンを使用し
て、検量線を作成した。 （使用ポリスチレン） ・東ソー株式会社製 標準ポリスチレン （詳細表１掲
載）(1) Weight average molecular weight and molecular weight distribution Gel permeation chromatography (GPC
Method) and the measurement was carried out in terms of polystyrene. That is, as GPC filler, Shodex GPCA-
A 1.5 cm ID, 46 cm long column packed with 804 is used. First, a calibration curve was prepared using the following standard polystyrene. (Polystyrene used)-Standard polystyrene manufactured by Tosoh Corporation (Detailed Table 1)
【００３６】[0036]
【表１】 [Table 1]
【００３７】すなわち、カラム温度を約２０℃に保持し
た状態で、表１の標準ポリスチレン試料３０ｍｇをテト
ラヒドロフラン５ｍｌに溶解した溶液４５μｌを注入
し、１.０ｍｌ／分の速度でテトラヒドロフランを流し
て、ウォーターズ社製４８６型ディテクターを使用して
２５４ｎｍの紫外線によって検出する。That is, while maintaining the column temperature at about 20 ° C., 45 μl of a solution prepared by dissolving 30 mg of the standard polystyrene sample shown in Table 1 in 5 ml of tetrahydrofuran was injected, and tetrahydrofuran was flowed at a rate of 1.0 ml / min. Detection is carried out with 254 nm ultraviolet light using a 486 type detector manufactured by KK.
【００３８】次に、製造したポリカーボネート樹脂につ
いても同様の操作にて測定し、その結果を先程のポリス
チレン検量線と対応させることにより、分子量分布を決
定した。Next, the produced polycarbonate resin was measured in the same manner, and the molecular weight distribution was determined by associating the result with the above-mentioned polystyrene calibration curve.
【００３９】（２）転写性 射出成形機（名機製作所 Ｍ３５Ｂ−Ｄ−ＤＭ）とキャ
ビティ厚０.６ｍｍｔ直径１２０ｍｍの金型および深さ
１４５ｎｍ幅０.７４μｍの溝が刻まれたスタンパーを
用いて、金型温度１２５℃、充填時間０.２秒、冷却時
間１５秒、型締力３５トンでディスク基板を成形した。
次に原子間力顕微鏡（セイコー電子工業ＳＰＩ３７０
０）にてｒ＝５５ｍｍにおけるディスク基板の溝部の深
さを測定し、溝形状の再現率（＝１００×ディスクの溝
深さ／スタンパーの溝深さ（％））を求めた。また成形
した基板を１０００枚目視観察し、割れの有無を確認し
た。(2) Transferability Using an injection molding machine (Meiki Seisakusho M35BD-DM), a mold having a cavity thickness of 0.6 mmt and a diameter of 120 mm, and a stamper having a groove having a depth of 145 nm and a width of 0.74 μm. A disk substrate was formed at a mold temperature of 125 ° C., a filling time of 0.2 seconds, a cooling time of 15 seconds, and a clamping force of 35 tons.
Next, an atomic force microscope (Seiko Electronics Industries SPI370
At 0), the depth of the groove of the disk substrate at r = 55 mm was measured, and the reproducibility of the groove shape (= 100 × groove depth of disk / groove depth of stamper (%)) was determined. In addition, 1,000 molded substrates were visually observed to check for cracks.
【００４０】実施例１ 温度計、撹拌機および還流冷却器付き反応器にイオン交
換水４３５部、４８％水酸化ナトリウム水溶液７９.６
部を仕込み、これに２,２−ビス（４−ヒドロキシフェ
ニル）プロパン１１４部およびハイドロサルファイト
０.２３部を溶解した後、塩化メチレン３５９部を加
え、撹拌下１５〜２５℃でホスゲン５６.２部を４０分
要して吹込んだ。ホスゲン吹き込み終了後、４８％水酸
化ナトリウム水溶液１４.３部およびｐ−ｔｅｒｔ−ブ
チルフェノール３.９部を加え、撹拌を始め、乳化後ト
リエチルアミン０.１２部を加え、さらに２８〜３３℃
で１時間撹拌して反応を終了した。反応終了後生成物を
塩化メチレン９６８部で希釈して水洗した後塩酸酸性に
して水洗し、水相の導電率がイオン交換水と殆ど同じに
なるまで水洗を繰り返して、重量平均分子量２４,１０
０であるポリカーボネートの塩化メチレン溶液を得た。
この塩化メチレン溶液にアセトン８３６部を加えた後、
さらに３０分攪拌して析出分を十分に熟成した後、析出
分のポリカーボネート樹脂を濾取して、低分子量成分を
除去したパウダーを得た。このパウダーにトリス（２,
４−ｄｉ−ｔｅｒｔ−ブチルフェニル）ホスファイトを
０.００２５重量％、ステアリン酸モノグリセリドを０.
０５重量％加えた。次に、かかるパウダーをベント式二
軸押出機［神戸製鋼（株）製ＫＴＸ−４６］によりシリ
ンダー温度２４０℃で脱気しながら溶融混練し、重量平
均分子量３０,８００のペレットを得た。この時の重量
平均分子量および各分子量水準の構成比ならびに成形評
価結果を、表２に掲載した。Example 1 A reactor equipped with a thermometer, a stirrer and a reflux condenser was charged with 435 parts of ion-exchanged water and 79.6% aqueous 48% sodium hydroxide solution.
After dissolving 114 parts of 2,2-bis (4-hydroxyphenyl) propane and 0.23 part of hydrosulfite, 359 parts of methylene chloride was added thereto, and phosgene 56. I took two parts for 40 minutes. After completion of the phosgene blowing, 14.3 parts of a 48% aqueous sodium hydroxide solution and 3.9 parts of p-tert-butylphenol were added, stirring was started, and after emulsification, 0.12 parts of triethylamine was added.
For 1 hour to complete the reaction. After completion of the reaction, the product was diluted with 968 parts of methylene chloride, washed with water, acidified with hydrochloric acid, washed with water, and repeatedly washed with water until the conductivity of the aqueous phase became almost the same as that of ion-exchanged water.
Thus, a methylene chloride solution of the polycarbonate was obtained.
After adding 836 parts of acetone to this methylene chloride solution,
After stirring for further 30 minutes to sufficiently mature the precipitate, the precipitated polycarbonate resin was collected by filtration to obtain a powder from which low molecular weight components had been removed. Tris (2,
0.0025% by weight of 4-di-tert-butylphenyl) phosphite and 0.2% by weight of stearic acid monoglyceride.
05% by weight was added. Next, the powder was melt-kneaded with a vented twin-screw extruder [KTX-46 manufactured by Kobe Steel Ltd.] at a cylinder temperature of 240 ° C. to obtain pellets having a weight average molecular weight of 30,800. Table 2 shows the weight average molecular weight, the composition ratio of each molecular weight level, and the molding evaluation results at this time.
【００４１】実施例２ イオン交換水６０９部、４８％水酸化ナトリウム水溶液
１１２部を仕込み、これに２,２−ビス（４−ヒドロキ
シフェニル）プロパン１６０部およびハイドロサルファ
イト０.３２部を溶解した後、塩化メチレン５０２部を
加え、撹拌下１５〜２５℃でホスゲン７８.６部を４０
分要して吹込んだ。ホスゲン吹き込み終了後、４８％水
酸化ナトリウム水溶液２０.０部およびｐ−ｔｅｒｔ−
ブチルフェノール６.６部を加え、撹拌を始め、乳化後
トリエチルアミン５.０部を加え、さらに２８〜３３℃
で１時間撹拌して反応を終了した。反応終了後生成物を
塩化メチレン１３６０部で希釈して水洗した後塩酸酸性
にして水洗し、水相の導電率がイオン交換水とほとんど
同じになるまで水洗を繰返して、重量平均分子量２７,
５００であるポリカーボネートの塩化メチレン溶液を得
た。この塩化メチレン溶液にアセトン４１１部を加えた
直後に析出してくる高分子量成分が多く含まれるポリカ
ーボネートの析出分を濾過により除去した。この濾過板
を通過した溶液について、さらに３０分攪拌して再び析
出してくるポリカーボネートを十分に熟成した後、今度
は析出分のポリカーボネート樹脂を濾取して、低分子量
成分を除去したパウダーを得た。以下、実施例１と同様
な方法で、重量平均分子量２９,６００のペレットを得
た。この時の重量平均分子量および各分子量水準の構成
比ならびに成形評価結果を、表２に掲載した。Example 2 609 parts of ion-exchanged water and 112 parts of a 48% aqueous sodium hydroxide solution were charged, and 160 parts of 2,2-bis (4-hydroxyphenyl) propane and 0.32 parts of hydrosulfite were dissolved therein. Thereafter, 502 parts of methylene chloride was added, and 78.6 parts of phosgene was added at 15 to 25 ° C. with stirring.
I blew it in a minute. After the phosgene blowing was completed, 20.0 parts of a 48% aqueous sodium hydroxide solution and p-tert-
6.6 parts of butylphenol were added, stirring was started, and after emulsification, 5.0 parts of triethylamine was added.
For 1 hour to complete the reaction. After completion of the reaction, the product was diluted with 1360 parts of methylene chloride, washed with water, acidified with hydrochloric acid, washed with water, and repeatedly washed with water until the conductivity of the aqueous phase became almost the same as that of ion-exchanged water.
A methylene chloride solution of polycarbonate of 500 was obtained. Immediately after adding 411 parts of acetone to this methylene chloride solution, a polycarbonate precipitate containing a large amount of high molecular weight components, which was precipitated, was removed by filtration. The solution passed through the filter plate was further stirred for 30 minutes to sufficiently mature the precipitated polycarbonate, and then the precipitated polycarbonate resin was filtered to obtain a powder from which low molecular weight components had been removed. Was. Thereafter, in the same manner as in Example 1, pellets having a weight average molecular weight of 29,600 were obtained. Table 2 shows the weight average molecular weight, the composition ratio of each molecular weight level, and the molding evaluation results at this time.
【００４２】実施例３ 撹拌機および蒸留塔を備えた反応器に２,２−ビス（４
−ヒドロキシフェニル）プロパン５０５部、ジフェニル
カーボネート（バイエル社製）４９３部および触媒とし
て水酸化ナトリウム０.００００５部とテトラメチルア
ンモニウムヒドロキシド０.０１６部を仕込み、窒素置
換した。この混合物を２００℃まで加熱して撹拌しなが
ら溶解させた。次いで、減圧度を４０００Ｐａとして加
熱しながら１時間で大半のフェノールを留去し、更に２
７０℃まで温度を上げ、減圧度を１３３Ｐａとして２時
間重合反応を行ったところで、末端停止剤２−メトキシ
カルボニルフェニルフェニルカーボネート２３.０部を
添加した。その後２７０℃、１３３Ｐａ以下で５分間末
端封鎖反応を行った。次に溶融状態のままで、触媒中和
剤としてドデシルベンゼンスルホン酸テトラブチルホス
ホニウム塩を０.０２３部（４×１０-5モル／ビスフェ
ノール１モル）添加して２７０℃、１３３０Ｐａ以下で
１０分間反応を継続し、重量平均分子量２７,２００の
ポリマーを得た。このポリマー２５部を塩化メチレン２
６２部に加温溶解し、均一な溶液を得た。この溶液にア
セトン１６５部を加え以下、実施例２と同様な方法で重
量平均分子量２９,３００のペレットを得た。この時の
重量平均分子量および各分子量水準の構成比ならびに成
形評価結果を、表２に掲載した。Example 3 A reactor equipped with a stirrer and a distillation column was charged with 2,2-bis (4
-Hydroxyphenyl) propane (505 parts), diphenyl carbonate (manufactured by Bayer Co., Ltd.) (493 parts), sodium hydroxide (0.00005 part) and tetramethylammonium hydroxide (0.016 part) were charged and purged with nitrogen. This mixture was heated to 200 ° C. and dissolved with stirring. Next, most of the phenol was distilled off in 1 hour while heating at a reduced pressure of 4000 Pa.
After the temperature was raised to 70 ° C. and the polymerization reaction was carried out for 2 hours at a reduced pressure of 133 Pa, 23.0 parts of a terminal stopper 2-methoxycarbonylphenylphenyl carbonate were added. Thereafter, a terminal blocking reaction was performed at 270 ° C. and 133 Pa or less for 5 minutes. Next, in the molten state, 0.023 parts (4 × 10 −5 mol / 1 mol of bisphenol) of tetradecylphosphonium dodecylbenzenesulfonate as a catalyst neutralizing agent is added, and the mixture is reacted at 270 ° C. and 1330 Pa or less for 10 minutes. Was continued to obtain a polymer having a weight average molecular weight of 27,200. 25 parts of this polymer was treated with methylene chloride 2
The solution was heated and dissolved in 62 parts to obtain a uniform solution. 165 parts of acetone were added to this solution, and pellets having a weight average molecular weight of 29,300 were obtained in the same manner as in Example 2 below. Table 2 shows the weight average molecular weight, the composition ratio of each molecular weight level, and the molding evaluation results at this time.
【００４３】比較例１ 温度計、撹拌機および還流冷却器付き反応器にイオン交
換水３７４部、４８％水酸化ナトリウム水溶液６８.５
部を仕込み、これに２,２−ビス（４−ヒドロキシフェ
ニル）プロパン９８.０部およびハイドロサルファイト
０.２０部を溶解した後、塩化メチレン３０９部を加
え、撹拌下１５〜２５℃でホスゲン４８.３部を４０分
要して吹込んだ。ホスゲン吹き込み終了後、４８％水酸
化ナトリウム水溶液１２.３部およびｐ−ｔｅｒｔ−ブ
チルフェノール０.９５部を加え、撹拌を始め、乳化後
トリエチルアミン０.１０部を加え、さらに２８〜３３
℃で１時間撹拌して反応を終了し、重量平均分子量３
８,７００のポリカーボネート樹脂の塩化メチレン溶液
を得た。ｐ−ｔｅｒｔ−ブチルフェノールを４.０８部
加えた以外は上記と同様の方法で、重量平均分子量２
９,４００のポリカーボネート樹脂の塩化メチレン溶液
を得た。この２水準のポリカーボネート樹脂の塩化メチ
レン溶液について、ポリカーボネート樹脂重量比が、５
０／５０（ｗｔ％）になるように混合した後、軸受け部
に異物取出口を有する隔離室を設けたニーダー中の温水
にポリカーボネート樹脂溶液を滴下し、塩化メチレンを
留去しながらポリカーボネート樹脂樹脂をフレーク化し
た。次にこの含液ポリカーボネート樹脂を粉砕、乾燥し
て、重量平均分子３４,１００のパウダーを得た以外は
実施例１と同様におこなった。この時の重量平均分子量
および各分子量水準の構成比ならびに成形評価結果を、
表２に掲載した。Comparative Example 1 A reactor equipped with a thermometer, a stirrer and a reflux condenser was charged with 374 parts of ion-exchanged water and 68.5% of a 48% aqueous sodium hydroxide solution.
After dissolving 98.0 parts of 2,2-bis (4-hydroxyphenyl) propane and 0.20 parts of hydrosulfite, 309 parts of methylene chloride was added thereto, and phosgene was added at 15 to 25 ° C under stirring. 48.3 parts were blown in for 40 minutes. After completion of the phosgene blowing, 12.3 parts of a 48% aqueous sodium hydroxide solution and 0.95 parts of p-tert-butylphenol were added, stirring was started, and after emulsification, 0.10 parts of triethylamine was added.
C. for 1 hour to complete the reaction.
A methylene chloride solution of 8,700 polycarbonate resin was obtained. A weight-average molecular weight of 2 was obtained in the same manner as described above except that 4.08 parts of p-tert-butylphenol was added.
A 9,400 solution of the polycarbonate resin in methylene chloride was obtained. For the methylene chloride solution of these two levels of polycarbonate resin, the polycarbonate resin weight ratio is 5
0/50 (wt%), the polycarbonate resin solution was dropped into warm water in a kneader provided with an isolation chamber having a foreign substance take-out port in the bearing portion, and methylene chloride was distilled off to remove the polycarbonate resin solution. Was flaked. Next, this liquid-containing polycarbonate resin was pulverized and dried to obtain a powder having a weight average molecular weight of 34,100. At this time, the weight average molecular weight and the composition ratio of each molecular weight level and the molding evaluation results are as follows:
It is listed in Table 2.
【００４４】比較例２ 温度計、撹拌機および還流冷却器付き反応器にイオン交
換水８２７部、４８％水酸化ナトリウム水溶液１５１部
を仕込み、これに２,２−ビス（４−ヒドロキシフェニ
ル）プロパン２１７部およびハイドロサルファイト０.
４４部を溶解した後、塩化メチレン６８２部を加え、撹
拌下１５〜２５℃でホスゲン１０７部を４０分要して吹
込んだ。ホスゲン吹き込み終了後、４８％水酸化ナトリ
ウム水溶液２７.１部およびｐ−ｔｅｒｔ−ブチルフェ
ノール９.９０部を加え、撹拌を始め、乳化後トリエチ
ルアミン０.２２部を加え、さらに２８〜３３℃で１時
間撹拌して反応を終了して、重量平均分子量２２,９０
０のパウダーを得た以外は実施例１と同様におこなっ
た。この時の重量平均分子量および各分子量水準の構成
比ならびに成形評価結果を、表２に掲載した。COMPARATIVE EXAMPLE 2 A reactor equipped with a thermometer, a stirrer and a reflux condenser was charged with 827 parts of ion-exchanged water and 151 parts of a 48% aqueous sodium hydroxide solution, and charged with 2,2-bis (4-hydroxyphenyl) propane. 217 parts and hydrosulfite 0.1
After dissolving 44 parts, 682 parts of methylene chloride were added, and 107 parts of phosgene was blown in at 15 to 25 ° C for 40 minutes while stirring. After the completion of the phosgene blowing, 27.1 parts of a 48% aqueous sodium hydroxide solution and 9.90 parts of p-tert-butylphenol were added, stirring was started, and after emulsification, 0.22 parts of triethylamine was added. The reaction was terminated by stirring, and the weight average molecular weight was 22,90.
The procedure was performed in the same manner as in Example 1 except that a powder of 0 was obtained. Table 2 shows the weight average molecular weight, the composition ratio of each molecular weight level, and the molding evaluation results at this time.
【００４５】[0045]
【表２】 [Table 2]
【００４６】[0046]
【発明の効果】本発明の高精密転写性ポリカーボネート
樹脂光学用成形材料は、ポリカーボネート樹脂を成形し
てなる光記録媒体、とりわけ高密度記録媒体の製造に関
して、スタンパー形状に対する精密転写性、ハイサイク
ル成形性に好適であり、且つ、スタンパーへの付着物を
極めて抑制した高精密転写性ポリカーボネート樹脂光学
用成形材料として好適に用いられる。Industrial Applicability The high precision transferable polycarbonate resin optical molding material of the present invention relates to the production of an optical recording medium formed by molding a polycarbonate resin, in particular, a high density recording medium. It is suitably used as a molding material for high precision transferable polycarbonate resin optics, which is suitable for the properties and extremely suppresses the attachment to the stamper.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 藤丸 滋樹 東京都千代田区内幸町１丁目２番２号 帝 人化成株式会社内 Ｆターム(参考） 4J029 AA10 AB07 AC01 AC02 AD01 AE05 BB04B BB05A BB05B BB10A BB12A BB12B BB12C BB13A BB13B BC09 BD09A BD09C BG08X BH02 HC01 HC02 HC03 KE05 KE11 5D029 KA07 ────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Shigeki Fujimaru 1-2-2 Uchisaiwai-cho, Chiyoda-ku, Tokyo F-term in Teijin Chemicals Limited (Reference) 4J029 AA10 AB07 AC01 AC02 AD01 AE05 BB04B BB05A BB05B BB10A BB12A BB12B BB12C BB13A BB13B BC09 BD09A BD09C BG08X BH02 HC01 HC02 HC03 KE05 KE11 5D029 KA07
Claims (3)
ー法（ＧＰＣ法）により測定される重量平均分子量が、
２４,０００〜４０,０００のポリカーボネート樹脂であ
って、該ポリカーボネート樹脂中に含まれる分子量が１
０,０００以下のポリカーボネート化合物成分が９〜２
６重量％の範囲であり、かつ６０,０００以上のポリカ
ーボネート化合物成分が１２重量％以下であることを特
徴とする高精密転写性ポリカーボネート樹脂光学用成形
材料。The weight average molecular weight measured by gel permeation chromatography (GPC method) is as follows:
A polycarbonate resin having a molecular weight of 14,000 to 24,000 to 40,000.
9 to 2 polycarbonate component components of not more than 000
A high-precision transferable polycarbonate resin optical molding material having a content of 6% by weight and a polycarbonate compound component of 60,000 or more and 12% by weight or less.
２,２’−ビス（４−ヒドロキシフェニル）プロパンを
二価フェノール成分とする重縮合化合物である請求項１
記載の高精密転写性ポリカーボネート樹脂光学用成形材
料。2. The aromatic polycarbonate resin,
2. A polycondensation compound comprising 2,2'-bis (4-hydroxyphenyl) propane as a dihydric phenol component.
The high-precision transferable polycarbonate resin molding material described in the above.
により形成された光ディスク基板。3. An optical disk substrate formed of the aromatic polycarbonate resin according to claim 1.
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