JP2010202751A - Molded article comprising conductive resin composition - Google Patents
Molded article comprising conductive resin composition Download PDFInfo
- Publication number
- JP2010202751A JP2010202751A JP2009049203A JP2009049203A JP2010202751A JP 2010202751 A JP2010202751 A JP 2010202751A JP 2009049203 A JP2009049203 A JP 2009049203A JP 2009049203 A JP2009049203 A JP 2009049203A JP 2010202751 A JP2010202751 A JP 2010202751A
- Authority
- JP
- Japan
- Prior art keywords
- component
- resin composition
- molded article
- weight
- conductive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000011342 resin composition Substances 0.000 title claims abstract description 45
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 74
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 43
- 229920005989 resin Polymers 0.000 claims abstract description 34
- 239000011347 resin Substances 0.000 claims abstract description 34
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 26
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 26
- 239000011521 glass Substances 0.000 claims abstract description 24
- 125000003118 aryl group Chemical group 0.000 claims abstract description 20
- 229920005668 polycarbonate resin Polymers 0.000 claims abstract description 9
- 239000004431 polycarbonate resin Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 13
- 239000003365 glass fiber Substances 0.000 claims description 12
- 239000002041 carbon nanotube Substances 0.000 claims description 11
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 11
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 5
- 238000012546 transfer Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 230000003068 static effect Effects 0.000 abstract description 11
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 229920000515 polycarbonate Polymers 0.000 description 21
- 239000004417 polycarbonate Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 16
- 238000000465 moulding Methods 0.000 description 15
- 239000007789 gas Substances 0.000 description 14
- 238000002156 mixing Methods 0.000 description 14
- 239000008188 pellet Substances 0.000 description 14
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 10
- 238000001746 injection moulding Methods 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 239000000155 melt Substances 0.000 description 9
- 235000006708 antioxidants Nutrition 0.000 description 8
- 229920001577 copolymer Polymers 0.000 description 8
- 150000001491 aromatic compounds Chemical class 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000005809 transesterification reaction Methods 0.000 description 7
- 125000004203 4-hydroxyphenyl group Chemical group [H]OC1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 150000002989 phenols Chemical class 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 239000003381 stabilizer Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 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 5
- 239000011248 coating agent Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical class OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000007983 Tris buffer Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 230000001588 bifunctional effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- AIBRSVLEQRWAEG-UHFFFAOYSA-N 3,9-bis(2,4-ditert-butylphenoxy)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP1OCC2(COP(OC=3C(=CC(=CC=3)C(C)(C)C)C(C)(C)C)OC2)CO1 AIBRSVLEQRWAEG-UHFFFAOYSA-N 0.000 description 3
- BRPSWMCDEYMRPE-UHFFFAOYSA-N 4-[1,1-bis(4-hydroxyphenyl)ethyl]phenol Chemical compound C=1C=C(O)C=CC=1C(C=1C=CC(O)=CC=1)(C)C1=CC=C(O)C=C1 BRPSWMCDEYMRPE-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000009503 electrostatic coating Methods 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000003273 ketjen black Substances 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XRBCRPZXSCBRTK-UHFFFAOYSA-N phosphonous acid Chemical class OPO XRBCRPZXSCBRTK-UHFFFAOYSA-N 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- 150000003568 thioethers Chemical class 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical compound OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 description 2
- CUAWUNQAIYJWQT-UHFFFAOYSA-N 4-[1,1-bis(4-hydroxy-3,5-dimethylphenyl)ethyl]-2,6-dimethylphenol Chemical compound CC1=C(O)C(C)=CC(C(C)(C=2C=C(C)C(O)=C(C)C=2)C=2C=C(C)C(O)=C(C)C=2)=C1 CUAWUNQAIYJWQT-UHFFFAOYSA-N 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- GZOPWQQGCCGHDC-UHFFFAOYSA-N C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C Chemical compound C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C.C=C(C(=O)O)CC1=CC(=C(C(=C1)C)O)C(C)(C)C GZOPWQQGCCGHDC-UHFFFAOYSA-N 0.000 description 2
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-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
- 238000012695 Interfacial polymerization Methods 0.000 description 2
- XAQKFOUWWAKVCH-UHFFFAOYSA-N OP(O)OP(O)O.C(C)(C)(C1=CC=CC=C1)C1=C(C=CC(=C1)C(C)(C)C1=CC=CC=C1)C(O)C(CO)(CO)CO Chemical compound OP(O)OP(O)O.C(C)(C)(C1=CC=CC=C1)C1=C(C=CC(=C1)C(C)(C)C1=CC=CC=C1)C(O)C(CO)(CO)CO XAQKFOUWWAKVCH-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- CGRTZESQZZGAAU-UHFFFAOYSA-N [2-[3-[1-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]-2-methylpropan-2-yl]-2,4,8,10-tetraoxaspiro[5.5]undecan-9-yl]-2-methylpropyl] 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCC(C)(C)C2OCC3(CO2)COC(OC3)C(C)(C)COC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 CGRTZESQZZGAAU-UHFFFAOYSA-N 0.000 description 2
- BEIOEBMXPVYLRY-UHFFFAOYSA-N [4-[4-bis(2,4-ditert-butylphenoxy)phosphanylphenyl]phenyl]-bis(2,4-ditert-butylphenoxy)phosphane Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(C=1C=CC(=CC=1)C=1C=CC(=CC=1)P(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)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 BEIOEBMXPVYLRY-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000000071 blow moulding Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- ZJIPHXXDPROMEF-UHFFFAOYSA-N dihydroxyphosphanyl dihydrogen phosphite Chemical compound OP(O)OP(O)O ZJIPHXXDPROMEF-UHFFFAOYSA-N 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000010097 foam moulding Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 2
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 230000007257 malfunction Effects 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- BNJOQKFENDDGSC-UHFFFAOYSA-N octadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCC(O)=O BNJOQKFENDDGSC-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical class [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 2
- 229920001281 polyalkylene Polymers 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229920005990 polystyrene resin Polymers 0.000 description 2
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- HQHCYKULIHKCEB-UHFFFAOYSA-N tetradecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCC(O)=O HQHCYKULIHKCEB-UHFFFAOYSA-N 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- LZFOPEXOUVTGJS-ONEGZZNKSA-N trans-sinapyl alcohol Chemical compound COC1=CC(\C=C\CO)=CC(OC)=C1O LZFOPEXOUVTGJS-ONEGZZNKSA-N 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 2
- FEODVXCWZVOEIR-UHFFFAOYSA-N (2,4-ditert-butylphenyl) octyl hydrogen phosphite Chemical compound CCCCCCCCOP(O)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C FEODVXCWZVOEIR-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
- PHJMLWHPHSYYQI-UHFFFAOYSA-N 1,1-bis(2,6-ditert-butyl-4-ethylphenyl)-2,2-bis(hydroxymethyl)propane-1,3-diol dihydroxyphosphanyl dihydrogen phosphite Chemical compound OP(O)OP(O)O.C(C)(C)(C)C1=C(C(=CC(=C1)CC)C(C)(C)C)C(O)(C(CO)(CO)CO)C1=C(C=C(C=C1C(C)(C)C)CC)C(C)(C)C PHJMLWHPHSYYQI-UHFFFAOYSA-N 0.000 description 1
- NVWZUUBHBWBVAE-UHFFFAOYSA-N 1,2,3,4-tetrakis(2,4-ditert-butylphenyl)biphenylene Chemical group CC(C)(C)C1=CC(C(C)(C)C)=CC=C1C(C(=C1C=2C(=CC(=CC=2)C(C)(C)C)C(C)(C)C)C=2C(=CC(=CC=2)C(C)(C)C)C(C)(C)C)=C(C=2C3=CC=CC=2)C3=C1C1=CC=C(C(C)(C)C)C=C1C(C)(C)C NVWZUUBHBWBVAE-UHFFFAOYSA-N 0.000 description 1
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- VNQNXQYZMPJLQX-UHFFFAOYSA-N 1,3,5-tris[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-1,3,5-triazinane-2,4,6-trione Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CN2C(N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C(=O)N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C2=O)=O)=C1 VNQNXQYZMPJLQX-UHFFFAOYSA-N 0.000 description 1
- OSZQBLPOQBBXQS-UHFFFAOYSA-N 1,3,7,9-tetratert-butyl-11-(2,4-ditert-butylphenoxy)-5h-benzo[d][1,3,2]benzodioxaphosphocine Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP1OC2=C(C(C)(C)C)C=C(C(C)(C)C)C=C2CC(C=C(C=C2C(C)(C)C)C(C)(C)C)=C2O1 OSZQBLPOQBBXQS-UHFFFAOYSA-N 0.000 description 1
- MRMCMJOXMLGUFT-UHFFFAOYSA-N 1,3,7,9-tetratert-butyl-11-(2-tert-butyl-4-methylphenoxy)-5h-benzo[d][1,3,2]benzodioxaphosphocine Chemical compound CC(C)(C)C1=CC(C)=CC=C1OP1OC2=C(C(C)(C)C)C=C(C(C)(C)C)C=C2CC(C=C(C=C2C(C)(C)C)C(C)(C)C)=C2O1 MRMCMJOXMLGUFT-UHFFFAOYSA-N 0.000 description 1
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 1
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- Manufacture Of Macromolecular Shaped Articles (AREA)
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Abstract
Description
本発明は、導電性樹脂組成物からなる成形品に関する。さらに詳しくは、本発明は、半導電性領域内に、成形品の表面抵抗率と帯電圧半減衰時間を制御することが可能であり、成形品表面から発生するスパーク電流を抑制し、成形品の樹脂表面から導電性炭素材料が脱落することを抑制し、更には寸法安定性、流動性、外観等にも優れた、半導体関連部材に適した導電性樹脂組成物からなる成形品に関する。 The present invention relates to a molded article made of a conductive resin composition. More specifically, the present invention can control the surface resistivity and the half voltage decay time of the molded product in the semiconductive region, suppress the spark current generated from the surface of the molded product, The present invention relates to a molded article made of a conductive resin composition suitable for a semiconductor-related member, which is excellent in dimensional stability, fluidity, appearance and the like.
ハードディスク関連部品およびその工程内容器、ICチップトレイ、ウェハー搬送容器、ガラスコンテナ等で例示される半導体関連部材に対し、OA機器や電子機器の小型軽量化や、高集積化、高精度化の進行とともに、関連する工程内での塵やほこりの付着低減や、OA機器や電子機器の静電気障害による誤作動防止という要求が、年々厳しくなってきている。静電気障害による誤作動を防止するには、ハードディスク周辺での塵やほこりの付着を防ぎ、かつ障害の基となる静電気を溜めないよう、ハードディスク周辺の部品の表面抵抗率を105〜1012Ω/sqに制御することが通例である。また、自動車外装部品は、塗料の付着効率を向上させるために静電塗装が一般に行われている。静電塗装とは、アースした塗装物を陽極、塗装霧化装置を陰極とし、これに負の高電圧を与えて、両極間に静電界を作り、霧化した塗装粒子を負に帯電させて反対極である被塗物に効率よく塗料を吸着させる塗装方法である。熱可塑性樹脂は電気絶縁性であるため、静電塗装を行うには導電性の付与が必要であり、少量の導電性物質の配合で高い導電性を得るために導電性炭素材料を配合することが広く行われている。芳香族ポリカーボネートと熱可塑性ポリアルキレンフタレートとのアロイに導電性炭素材料を配合することは公知であり、特許文献1では芳香族ポリカーボネートと導電性カーボンブラックに熱可塑性ポリアルキレンフタレートを配合することで、ポリカーボネート樹脂の機械特性や成形加工性、更には導電性を損なうことなく、カーボンブラックの分散性を向上させている。また、特許文献2では、耐衝撃性、寸法安定性、流動性、外観等にも優れた導電性樹脂組成物を提供すべく、芳香族ポリカーボネートとポリエチレンテレフタレートとのアロイに導電性カーボンブラックを配合し、かつ導電性カーボンブラックの分散をポリエチレンテレフタレート相に偏在させることを提案している。しかしながら、これらの特許文献では成形品の表面抵抗率が例示されているが、これは通例の静電気障害対策であり、部材の小型軽量化や、高集積化、高精度化が進む中で、より厳しい静電気障害に対するユーザーの要求に応えていくには不十分である。現状では、万が一スパークが発生した場合でも精密部品が破壊に至らないようにスパーク電流を小さく抑えることが必要となってきている。また、導電性炭素材料は、成形品の樹脂表面からの脱落が問題とされており、新たな塵の発生源となるため、高レベルな静電気障害が要求される用途への展開に制限があった。
Progress in miniaturization and weight reduction of OA equipment and electronic equipment, high integration, and high precision for semiconductor-related members exemplified by hard disk-related parts and in-process containers, IC chip trays, wafer transfer containers, glass containers, etc. At the same time, demands for reducing the adhesion of dust and dust in related processes and preventing malfunctions due to static electricity failures of OA equipment and electronic equipment are becoming stricter year by year. In order to prevent malfunction due to static electricity failure, the surface resistivity of the components around the hard disk is set to 10 5 to 10 12 Ω so as to prevent dust and dust from adhering around the hard disk and to prevent static electricity that is the basis of the failure. It is customary to control to / sq. Moreover, electrostatic coating is generally performed on automobile exterior parts in order to improve the adhesion efficiency of paint. Electrostatic coating uses a grounded coating as an anode and a coating atomizer as a cathode. A negative high voltage is applied to this to create an electrostatic field between the two electrodes, and the atomized coating particles are charged negatively. This is a coating method in which a paint is efficiently adsorbed on an object that is the opposite pole. Since thermoplastic resin is electrically insulating, it is necessary to add conductivity to perform electrostatic coating. To obtain high conductivity with a small amount of conductive material, a conductive carbon material should be added. Is widely practiced. It is known to blend a conductive carbon material into an alloy of an aromatic polycarbonate and a thermoplastic polyalkylene phthalate, and in
本発明の目的は、半導電性領域内に、成形品の表面抵抗率と帯電圧半減衰時間を制御することで、成形品表面から発生するスパーク電流を抑制し、加えて成形品の樹脂表面から導電性炭素材料が脱落することを抑制し、更には寸法安定性、流動性、外観等にも優れた、半導体関連部材に適した導電性樹脂組成物からなる成形品を提供することにある。 The object of the present invention is to control the spark current generated from the surface of the molded product by controlling the surface resistivity and charged voltage half decay time of the molded product in the semiconductive region, and in addition to the resin surface of the molded product. It is intended to provide a molded article made of a conductive resin composition suitable for semiconductor-related members, which is excellent in dimensional stability, fluidity, appearance, etc. .
本発明者らは上記課題を解決するために、鋭意検討を重ねた結果、本発明を完成した。即ち、本発明者らは、芳香族ポリカーボネート樹脂55〜75重量%(A成分)およびポリエチレンテレフタレート樹脂25〜45重量%(B成分)からなる樹脂成分100重量部に対し、導電性炭素材料(C成分)を1〜20重量部含有させることにより、該導電性樹脂組成物からなる成形品の表面抵抗率を静電領域である105〜1012Ω/sqに制御することに加えて10kVを印加したときの半減衰時間を制御することにより、静電気障害の一つとなるスパーク電流をも低減させることができるという驚くべき効果を見出した。さらに、ポリエチレンテレフタレートの添加量を25〜45重量%という限られた範囲に限定した場合、より少ない導電性炭素材料の添加量で上記スパーク電流の低減という効力を発揮させることができ、加えて成形品の樹脂表面から導電性炭素材料が脱落することを抑制でき、且つポリエチレンテレフタレートの添加による寸法安定性の悪化を抑えられることを見出し、本発明を完成させた。 In order to solve the above-mentioned problems, the present inventors have intensively studied to complete the present invention. That is, the present inventors made conductive carbon material (C) with respect to 100 parts by weight of resin component consisting of 55 to 75% by weight (component A) of aromatic polycarbonate resin and 25 to 45% by weight (component B) of polyethylene terephthalate resin. In addition to controlling the surface resistivity of the molded article made of the conductive resin composition to 10 5 to 10 12 Ω / sq, which is an electrostatic region, by adding 1 to 20 parts by weight of the component) 10 kV The inventors have found a surprising effect that by controlling the half decay time when applied, it is possible to reduce the spark current that is one of the electrostatic disturbances. Furthermore, when the addition amount of polyethylene terephthalate is limited to a limited range of 25 to 45% by weight, the effect of reducing the spark current can be exhibited with a smaller addition amount of the conductive carbon material. It has been found that the conductive carbon material can be prevented from falling off from the resin surface of the product, and that the deterioration of dimensional stability due to the addition of polyethylene terephthalate can be suppressed, and the present invention has been completed.
スパーク電流が低減する機構は、導電性炭素材料が成形品の樹脂表面に微細分散し樹脂に溜まった静電気が導電性炭素材料へ迅速に移動するためスパーク電流が低減したものと考えられる。スパーク電流は電界誘導法で高電圧を印加した成形品に端子を近づけてスパークさせそのスパーク電流を測定する方法で測定でき、JEDEC規格(JESD22−C1010C)に準拠した方法である。成形品がより少ない導電性炭素材料の添加量で上記スパーク電流の低減という効力を発揮できるのは、導電性炭素材料がポリエチレンテレフタレートにのみ偏在するためと考えられる。成形品の樹脂表面からの導電性炭素材料の脱落がポリエチレンテレフタレートの配合により抑制できるのは、導電性炭素材料表面とポリエチレンテレフタレートとの馴染みが良いためと考えられる。 The mechanism by which the spark current is reduced is considered to be that the spark current is reduced because the conductive carbon material is finely dispersed on the resin surface of the molded product and the static electricity accumulated in the resin quickly moves to the conductive carbon material. The spark current can be measured by a method in which a terminal is brought close to a molded product to which a high voltage is applied by an electric field induction method and the spark current is measured, and is a method based on the JEDEC standard (JESD22-C1010C). The reason why the molded article can exhibit the effect of reducing the spark current with a smaller amount of the conductive carbon material added is presumably because the conductive carbon material is unevenly distributed only in polyethylene terephthalate. The reason why the conductive carbon material can be prevented from falling off from the resin surface of the molded product by blending polyethylene terephthalate is considered to be because the familiarity between the surface of the conductive carbon material and polyethylene terephthalate is good.
本発明の樹脂組成物からなる成形品は、静電気障害の一つとなるスパーク電流が小さく、導電性炭素材料の脱落も少なく、また好適な寸法安定性、流動性、外観等を有するため、ハードディスク関連部品およびその工程内容器、ICチップトレイ、ウェハー搬送容器、ガラスコンテナ、並びに自動車外装部品等に有用である。 The molded article made of the resin composition of the present invention has a small spark current, which is one of the static electricity obstacles, little drop of the conductive carbon material, and suitable dimensional stability, fluidity, appearance, etc. It is useful for parts and in-process containers, IC chip trays, wafer transfer containers, glass containers, automobile exterior parts, and the like.
<A成分:芳香族ポリカーボネート>
芳香族ポリカーボネート(A成分)とは、二価フェノールとカーボネート前駆体とを反応させて得られるものである。反応の方法としては界面重縮合法、溶融エステル交換法、カーボネートプレポリマーの固相エステル交換法、および環状カーボネート化合物の開環重合法などを挙げることができる。
<Component A: aromatic polycarbonate>
An aromatic polycarbonate (component A) is obtained by reacting a dihydric phenol and a carbonate precursor. Examples of the reaction method include an interfacial polycondensation method, a melt transesterification method, a solid phase transesterification method of a carbonate prepolymer, and a ring-opening polymerization method of a cyclic carbonate compound.
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’−ビフェノール、1,1−ビス(4−ヒドロキシフェニル)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−ヒドロキシフェニル)ブタン、1,1−ビス(4−ヒドロキシフェニル)−1−フェニルエタン、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)−3,3,5−トリメチルシクロヘキサン、2,2−ビス(4−ヒドロキシフェニル)ペンタン、4,4’−(p−フェニレンジイソプロピリデン)ジフェノール、4,4’−(m−フェニレンジイソプロピリデン)ジフェノール、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、ビス(4−ヒドロキシフェニル)オキシド、ビス(4−ヒドロキシフェニル)スルフィド、ビス(4−ヒドロキシフェニル)スルホキシド、ビス(4−ヒドロキシフェニル)スルホン、ビス(4−ヒドロキシフェニル)ケトン、ビス(4−ヒドロキシフェニル)エステル、ビス(4−ヒドロキシ−3−メチルフェニル)スルフィド、9,9−ビス(4−ヒドロキシフェニル)フルオレンおよび9,9−ビス(4−ヒドロキシ−3−メチルフェニル)フルオレンなどが挙げられる。好ましい二価フェノールは、ビス(4−ヒドロキシフェニル)アルカンであり、なかでも靭性に優れる点からビスフェノールA(以下“BPA”と略称することがある)が特に好ましく、汎用されている。 Representative examples of the dihydric phenol used here include hydroquinone, resorcinol, 4,4′-biphenol, 1,1-bis (4-hydroxyphenyl) ethane, and 2,2-bis (4-hydroxyphenyl). ) Propane (commonly called bisphenol A), 2,2-bis (4-hydroxy-3-methylphenyl) propane, 2,2-bis (4-hydroxyphenyl) butane, 1,1-bis (4-hydroxyphenyl)- 1-phenylethane, 1,1-bis (4-hydroxyphenyl) cyclohexane, 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane, 2,2-bis (4-hydroxyphenyl) Pentane, 4,4 ′-(p-phenylenediisopropylidene) diphenol, 4,4 ′-(m-phenylenediisopropyl Pyridene) diphenol, 1,1-bis (4-hydroxyphenyl) -4-isopropylcyclohexane, bis (4-hydroxyphenyl) oxide, bis (4-hydroxyphenyl) sulfide, bis (4-hydroxyphenyl) sulfoxide, bis (4-hydroxyphenyl) sulfone, bis (4-hydroxyphenyl) ketone, bis (4-hydroxyphenyl) ester, bis (4-hydroxy-3-methylphenyl) sulfide, 9,9-bis (4-hydroxyphenyl) Examples include fluorene and 9,9-bis (4-hydroxy-3-methylphenyl) fluorene. A preferred dihydric phenol is bis (4-hydroxyphenyl) alkane, and bisphenol A (hereinafter sometimes abbreviated as “BPA”) is particularly preferred because of its excellent toughness, and is widely used.
カーボネート前駆体としてはカルボニルハライド、炭酸ジエステルまたはハロホルメートなどが使用され、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などが挙げられる。 As the carbonate precursor, carbonyl halide, carbonic acid diester, haloformate or the like is used, and specific examples include phosgene, diphenyl carbonate, dihaloformate of dihydric phenol, and the like.
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によっ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、二価フェノールが酸化するのを防止するための酸化防止剤などを使用してもよい。また本発明の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、芳香族または脂肪族(脂環式を含む)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、二官能性アルコール(脂環式を含む)を共重合した共重合ポリカーボネート樹脂、並びにかかる二官能性カルボン酸および二官能性アルコールを共に共重合したポリエステルカーボネートを含む。また、得られたポリカーボネートの2種以上を混合した混合物であってもよい。 In producing a polycarbonate resin by interfacial polymerization of the above dihydric phenol and carbonate precursor, a catalyst, a terminal terminator, an antioxidant for preventing the dihydric phenol from being oxidized, etc., as necessary. May be used. The polycarbonate resin of the present invention is a branched polycarbonate resin copolymerized with a trifunctional or higher polyfunctional aromatic compound, or a polyester carbonate resin copolymerized with an aromatic or aliphatic (including alicyclic) difunctional carboxylic acid. , Copolymerized polycarbonate resins copolymerized with bifunctional alcohols (including alicyclic), and polyester carbonates copolymerized with such bifunctional carboxylic acids and difunctional alcohols. Moreover, the mixture which mixed 2 or more types of the obtained polycarbonate may be sufficient.
分岐ポリカーボネートは、本発明の樹脂組成物の溶融張力を増加させ、かかる特性に基づいて押出成形、発泡成形およびブロー成形における成形加工性を改善できる。結果として寸法精度により優れた、これらの成形法による成形品が得られる。 The branched polycarbonate increases the melt tension of the resin composition of the present invention, and can improve the molding processability in extrusion molding, foam molding and blow molding based on such properties. As a result, a molded product by these molding methods, which is superior in dimensional accuracy, is obtained.
かかる分岐ポリカーボネート樹脂に使用される三官能以上の多官能性芳香族化合物としては、4,6−ジメチル−2,4,6−トリス(4−ヒドロキジフェニル)ヘプテン−2、2,4,6−トリメチル−2,4,6−トリス(4−ヒドロキシフェニル)ヘプタン、1,3,5−トリス(4−ヒドロキシフェニル)ベンゼン、1,1,1−トリス(4−ヒドロキシフェニル)エタン、1,1,1−トリス(3,5−ジメチル−4−ヒドロキシフェニル)エタン、2,6−ビス(2−ヒドロキシ−5−メチルベンジル)−4−メチルフェノール、および4−{4−[1,1−ビス(4−ヒドロキシフェニル)エチル]ベンゼン}−α,α−ジメチルベンジルフェノール等のトリスフェノールが好適に例示される。その他多官能性芳香族化合物としては、フロログルシン、フロログルシド、テトラ(4−ヒドロキシフェニル)メタン、ビス(2,4−ジヒドロキシフェニル)ケトン、1,4−ビス(4,4−ジヒドロキシトリフェニルメチル)ベンゼン、並びにトリメリット酸、ピロメリット酸、ベンゾフェノンテトラカルボン酸およびこれらの酸クロライド等が例示される。中でも1,1,1−トリス(4−ヒドロキシフェニル)エタンおよび1,1,1−トリス(3,5−ジメチル−4−ヒドロキシフェニル)エタンが好ましく、特に1,1,1−トリス(4−ヒドロキシフェニル)エタンが好ましい。 Examples of the trifunctional or higher polyfunctional aromatic compound used in the branched polycarbonate resin include 4,6-dimethyl-2,4,6-tris (4-hydroxydiphenyl) heptene-2, 2,4,6- Trimethyl-2,4,6-tris (4-hydroxyphenyl) heptane, 1,3,5-tris (4-hydroxyphenyl) benzene, 1,1,1-tris (4-hydroxyphenyl) ethane, 1,1 , 1-tris (3,5-dimethyl-4-hydroxyphenyl) ethane, 2,6-bis (2-hydroxy-5-methylbenzyl) -4-methylphenol, and 4- {4- [1,1- Trisphenol such as bis (4-hydroxyphenyl) ethyl] benzene} -α, α-dimethylbenzylphenol is preferably exemplified. Other polyfunctional aromatic compounds include phloroglucin, phloroglucid, tetra (4-hydroxyphenyl) methane, bis (2,4-dihydroxyphenyl) ketone, 1,4-bis (4,4-dihydroxytriphenylmethyl) benzene. And trimellitic acid, pyromellitic acid, benzophenone tetracarboxylic acid, and acid chlorides thereof. Of these, 1,1,1-tris (4-hydroxyphenyl) ethane and 1,1,1-tris (3,5-dimethyl-4-hydroxyphenyl) ethane are preferable, and 1,1,1-tris (4- Hydroxyphenyl) ethane is preferred.
分岐ポリカーボネートにおける多官能性芳香族化合物から誘導される構成単位は、二価フェノールから誘導される構成単位とかかる多官能性芳香族化合物から誘導される構成単位との合計100モル部中、0.03〜1モル部、好ましくは0.07〜0.7モル部、特に好ましくは0.1〜0.4モル部である。 The structural unit derived from the polyfunctional aromatic compound in the branched polycarbonate is 0.1% in a total of 100 mole parts of the structural unit derived from the dihydric phenol and the structural unit derived from the polyfunctional aromatic compound. It is 03-1 mol part, Preferably it is 0.07-0.7 mol part, Most preferably, it is 0.1-0.4 mol part.
また、かかる分岐構造単位は、多官能性芳香族化合物から誘導されるだけでなく、溶融エステル交換反応時の副反応の如き、多官能性芳香族化合物を用いることなく誘導されるものであってもよい。尚、かかる分岐構造の割合については1H−NMR測定により算出することが可能である。 Further, such a branched structural unit is not only derived from a polyfunctional aromatic compound but also derived without using a polyfunctional aromatic compound, such as a side reaction during a melt transesterification reaction. Also good. The ratio of such a branched structure can be calculated by 1 H-NMR measurement.
一方、脂肪族の二官能性のカルボン酸は、α,ω−ジカルボン酸が好ましく、その具体例としては、セバシン酸(デカン二酸)、ドデカン二酸、テトラデカン二酸、オクタデカン二酸、イコサン二酸等の直鎖飽和脂肪族ジカルボン酸並びにシクロヘキサンジカルボン酸等の脂環族ジカルボン酸が挙げられる。二官能性アルコールとしては脂環族ジオールが好適であり、例えば、シクロヘキサンジメタノール、シクロヘキサンジオール、トリシクロデカンジメタノール等が例示される。さらに、ポリオルガノシロキサン単位を共重合したポリカーボネート−ポリオルガノシロキサン共重合体の使用も可能である。 On the other hand, the aliphatic bifunctional carboxylic acid is preferably α, ω-dicarboxylic acid, and specific examples thereof include sebacic acid (decanedioic acid), dodecanedioic acid, tetradecanedioic acid, octadecanedioic acid, icosane diacid. Examples thereof include linear saturated aliphatic dicarboxylic acids such as acids and alicyclic dicarboxylic acids such as cyclohexanedicarboxylic acid. As the bifunctional alcohol, an alicyclic diol is suitable, and examples thereof include cyclohexanedimethanol, cyclohexanediol, and tricyclodecane dimethanol. Further, a polycarbonate-polyorganosiloxane copolymer obtained by copolymerizing polyorganosiloxane units can also be used.
A成分は、二価フェノール成分の異なるポリカーボネート、分岐成分を含有するポリカーボネート、各種のポリエステルカーボネート、ポリカーボネート−ポリオルガノシロキサン共重合体等を2種以上混合したものであってもよい。さらに、製造法の異なるポリカーボネート、末端停止剤の異なるポリカーボネート等を2種以上混合したものを使用することもできる。本発明の芳香族ポリカーボネートの製造方法である界面重合法、溶融エステル交換法、カーボネートプレポリマーの固相エステル交換法、および環状カーボネート化合物の開環重合法などの反応形式は、各種の文献および特許公報などで良く知られている方法である。 The component A may be a mixture of two or more of polycarbonates having different dihydric phenol components, polycarbonates containing branched components, various polyester carbonates, polycarbonate-polyorganosiloxane copolymers, and the like. Furthermore, what mixed 2 or more types of polycarbonates from which a manufacturing method differs, a polycarbonate from which a terminal terminator differs, etc. can also be used. Reaction formats such as interfacial polymerization, melt transesterification, solid phase transesterification of carbonate prepolymers, and ring-opening polymerization of cyclic carbonate compounds, which are methods for producing the aromatic polycarbonate of the present invention, are various documents and patents. This is a well-known method in gazettes.
本発明のA成分の芳香族ポリカーボネートとしては、バージン原料だけでなく、使用済みの製品から再生された芳香族ポリカーボネート、いわゆるマテリアルリサイクルされた芳香族ポリカーボネートの使用も可能である。使用済みの製品としては防音壁、ガラス窓、透光屋根材、および自動車サンルーフなどに代表される各種グレージング材、風防や自動車ヘッドランプレンズなどの透明部材、水ボトルなどの容器、並びに光記録媒体などが好ましく挙げられる。これらは多量の添加剤や他樹脂などを含むことがなく、目的の品質が安定して得られやすい。殊に自動車ヘッドランプレンズや光記録媒体などは上記の粘度平均分子量のより好ましい条件を満足するため好ましい態様として挙げられる。尚、上記のバージン原料とは、その製造後に未だ市場において使用されていない原料である。 As the A component aromatic polycarbonate of the present invention, not only a virgin raw material but also an aromatic polycarbonate regenerated from a used product, that is, a so-called material recycled aromatic polycarbonate can be used. Used products include soundproof walls, glass windows, translucent roofing materials, various glazing materials represented by automobile sunroofs, transparent members such as windshields and automobile headlamp lenses, containers such as water bottles, and optical recording media Etc. are preferred. These do not contain a large amount of additives or other resins, and the desired quality is easily obtained stably. In particular, an automotive headlamp lens, an optical recording medium, and the like are preferred as preferred embodiments because they satisfy the more preferable conditions of the viscosity average molecular weight. In addition, said virgin raw material is a raw material which is not yet used in the market after the manufacture.
本発明の成形品における表面抵抗率は、樹脂組成物の流動性に大きく影響を受けるため、その調整方法の一つに流動性を制御する方法を取ることができる。芳香族ポリカーボネートの粘度平均分子量は、好ましくは1×104〜5×104、より好ましくは1.4×104〜3×104、更に好ましくは1.8×104〜2.5×104である。1×104〜5×104の範囲においては、特に良好な耐衝撃性と流動性との両立に優れ、樹脂組成物からなる成形品の表面抵抗率を静電領域に調整することが容易となる。更に最も好適には、1.9×104〜2.4×104である。尚、かかる粘度平均分子量はA成分全体として満足すればよく、分子量の異なる2種以上の混合物によりかかる範囲を満足するものを含む。 Since the surface resistivity in the molded product of the present invention is greatly influenced by the fluidity of the resin composition, a method for controlling the fluidity can be taken as one of the adjustment methods. The viscosity average molecular weight of the aromatic polycarbonate is preferably 1 × 10 4 to 5 × 10 4 , more preferably 1.4 × 10 4 to 3 × 10 4 , and still more preferably 1.8 × 10 4 to 2.5 ×. 10 is four. In the range of 1 × 10 4 to 5 × 10 4 , both excellent impact resistance and fluidity are particularly excellent, and it is easy to adjust the surface resistivity of the molded product made of the resin composition to the electrostatic region. It becomes. Most preferably, it is 1.9 × 10 4 to 2.4 × 10 4 . The viscosity average molecular weight may be satisfied as the whole component A, and includes those satisfying such a range by a mixture of two or more kinds having different molecular weights.
本発明でいう粘度平均分子量はまず次式にて算出される比粘度を塩化メチレン100mlに芳香族ポリカーボネート0.7gを20℃で溶解した溶液からオストワルド粘度計を用いて求め、
比粘度(ηSP)=(t−t0)/t0
[t0は塩化メチレンの落下秒数、tは試料溶液の落下秒数]
求められた比粘度を次式にて挿入して粘度平均分子量Mを求める。
ηSP/c=[η]+0.45×[η]2c(但し[η]は極限粘度)
[η]=1.23×10−4M0.83
c=0.7
The viscosity average molecular weight referred to in the present invention is first determined by using an Ostwald viscometer from a solution in which 0.7 g of aromatic polycarbonate is dissolved in 100 ml of methylene chloride at 20 ° C., and the specific viscosity calculated by the following formula:
Specific viscosity (η SP ) = (t−t 0 ) / t 0
[T 0 is methylene chloride falling seconds, t is sample solution falling seconds]
The obtained specific viscosity is inserted by the following equation to determine the viscosity average molecular weight M.
η SP /c=[η]+0.45×[η] 2 c (where [η] is the intrinsic viscosity)
[Η] = 1.23 × 10 −4 M 0.83
c = 0.7
<B成分:ポリエチレンテレフタレート>
ポリエチレンテレフタレート(B成分)とは、芳香族ジカルボン酸成分としてテレフタル酸を主成分とし、かつ、ジオール成分としてエチレングリコールを主成分とし、これらの縮合反応によって得られる飽和ポリエステル重合体又は共重合体であり、繰返し単位としてエチレンテレフタレート単位を好ましくは70モル%以上、より好ましくは80モル%以上含む熱可塑性ポリエステル樹脂である。ポリエチレンテレフタレート樹脂の製造は、常法に従い、チタン、ゲルマニウム、アンチモン等を含有する重縮合触媒の存在下に、加熱しながら前記のジカルボン酸成分とジオール成分とを反応させ、副生する水又は低級アルコールを系外に排出することにより行われる。例えば、ゲルマニウム系重合触媒としては、ゲルマニウムの酸化物、水酸化物、ハロゲン化物、アルコラート、フェノラート等が例示でき、更に具体的には、酸化ゲルマニウム、水酸化ゲルマニウム、四塩化ゲルマニウム、テトラメトキシゲルマニウム等が例示できる。このとき、バッチ法、連続式のいずれの重合方法を取ることも可能であり、固相重合により重合度を上げることも可能である。
<B component: polyethylene terephthalate>
Polyethylene terephthalate (component B) is a saturated polyester polymer or copolymer obtained by a condensation reaction of terephthalic acid as an aromatic dicarboxylic acid component and ethylene glycol as a diol component. Yes, it is a thermoplastic polyester resin containing ethylene terephthalate units as repeating units, preferably 70 mol% or more, more preferably 80 mol% or more. According to a conventional method, the polyethylene terephthalate resin is produced by reacting the dicarboxylic acid component and the diol component with heating in the presence of a polycondensation catalyst containing titanium, germanium, antimony, etc. It is performed by discharging alcohol out of the system. For example, germanium-based polymerization catalysts include germanium oxides, hydroxides, halides, alcoholates, phenolates, and the like. More specifically, germanium oxide, germanium hydroxide, germanium tetrachloride, tetramethoxygermanium, etc. Can be illustrated. At this time, either a batch method or a continuous polymerization method can be employed, and the degree of polymerization can be increased by solid phase polymerization.
また使用するポリエチレンテレフタレートの末端基構造は特に限定されるものではなく、末端基における水酸基とカルボキシル基の割合がほぼ同量の場合以外に、一方の割合が多い場合であってもよい。またかかる末端基に対して反応性を有する化合物を反応させる等により、それらの末端基が封止されているものであってもよい。 Moreover, the terminal group structure of the polyethylene terephthalate to be used is not particularly limited, and may be a case where the ratio of one of the hydroxyl groups and the carboxyl group in the terminal group is large other than the case where the ratio is almost the same. Moreover, those terminal groups may be sealed by reacting a compound having reactivity with such terminal groups.
また本発明では、従来公知の重縮合の前段階であるエステル交換反応において使用される、マンガン、亜鉛、カルシウム、マグネシウム等の化合物を併せて使用でき、およびエステル交換反応終了後にリン酸または亜リン酸の化合物等により、かかる触媒を失活させて重縮合することも可能である。 Further, in the present invention, compounds such as manganese, zinc, calcium, magnesium, etc., which are used in a transesterification reaction that is a prior stage of a conventionally known polycondensation, can be used in combination, and phosphoric acid or phosphorous after completion of the transesterification reaction. Such a catalyst can be deactivated and polycondensed with an acid compound or the like.
またポリエチレンテレフタレート(B成分)の分子量については特に制限されないが、樹脂組成物からなる成形品の表面抵抗率を制御するために好適な流動性を得るためには、o−クロロフェノールを溶媒として25℃で測定した固有粘度が、好ましくは0.4〜1.2、より好ましくは0.65〜1.15である。 Further, the molecular weight of polyethylene terephthalate (component B) is not particularly limited, but in order to obtain a suitable fluidity for controlling the surface resistivity of the molded article made of the resin composition, o-chlorophenol is used as a solvent. The intrinsic viscosity measured at ° C is preferably 0.4 to 1.2, more preferably 0.65 to 1.15.
かかるポリエチレンテレフタレート(B成分)の含有量は、芳香族ポリカーボネート(A成分)との合計100重量%当り、25〜45重量%であり、27〜43重量%が好ましく、29〜41重量%がより好ましく、30〜40重量%が最も好ましい。ポリエチレンテレフタレートを配合することによって、導電性炭素材料がポリエチレンテレフタレート相に偏在するため、より少ない導電性炭素材料の添加量で導電性を得ることができる。しかし、ポリエチレンテレフタレートの配合が25重量%より小さくなると、ポリエチレンテレフタレートの配合量が少ないために導電性炭素材料の脱落を抑制できなくなり好ましくない。45重量%を超えると、ポリエチレンテレフタレートが樹脂成分のほぼ半分を占めるため寸法安定性が劣るようになり、好ましくない。また、ポリエチレンテレフタレート相の導電性炭素材料が希釈され、かかる表面抵抗率は1012Ω/sq以上となり好ましくない。 The content of the polyethylene terephthalate (component B) is 25 to 45% by weight, preferably 27 to 43% by weight, more preferably 29 to 41% by weight based on 100% by weight in total with the aromatic polycarbonate (component A). Preferably, 30 to 40% by weight is most preferable. By blending polyethylene terephthalate, the conductive carbon material is unevenly distributed in the polyethylene terephthalate phase, and therefore conductivity can be obtained with a smaller amount of the conductive carbon material added. However, if the blending ratio of polyethylene terephthalate is less than 25% by weight, the blending amount of polyethylene terephthalate is so small that it is not preferable because dropping of the conductive carbon material cannot be suppressed. If it exceeds 45% by weight, the polyethylene terephthalate accounts for almost half of the resin component, so that the dimensional stability becomes inferior. Moreover, the conductive carbon material of a polyethylene terephthalate phase is diluted, and this surface resistivity becomes 10 12 Ω / sq or more, which is not preferable.
<C成分:導電性炭素材料>
導電性炭素材料(C成分)は、樹脂組成物に導電性を付与し、導電性樹脂組成物からなる成形品の表面抵抗率と帯電半減衰時間を制御するために配合するものである。
導電性炭素材料としては、カーボンブラック、カーボンナノチューブ、無定形炭素、グラファイト、繊維状炭素、ナノカーボン等が挙げられるが、これらの中でもアウトガス、表面仕上がりおよび光沢性、流動性、スパーク電流等の点から、導電性カーボンブラック、カーボンナノチューブが好ましい。
<C component: conductive carbon material>
The conductive carbon material (component C) is blended to impart conductivity to the resin composition and to control the surface resistivity and charging half decay time of a molded product made of the conductive resin composition.
Examples of conductive carbon materials include carbon black, carbon nanotubes, amorphous carbon, graphite, fibrous carbon, and nanocarbon. Among these, outgas, surface finish and gloss, fluidity, spark current, etc. Therefore, conductive carbon black and carbon nanotube are preferable.
(導電性カーボンブラック)
導電性カーボンブラックとしては、ケッチェンブラック、アセチレンブラック、ファーネスブラック、サーマルブラック等が挙げられるが、これらの中でも従来の導電性カーボンブラックと比較して極少量で優れた導電性を示し、少量の添加で優れた導電性が得られる点で、ケッチェンブラックが好ましい。
(Conductive carbon black)
Examples of the conductive carbon black include ketjen black, acetylene black, furnace black, thermal black, etc. Among them, the conductive carbon black exhibits excellent conductivity in a very small amount compared to the conventional conductive carbon black, and a small amount Ketjen black is preferable in that excellent conductivity can be obtained by addition.
この導電性カーボンブラックは、特に原料、製法に制限されるものではないが、そのDBP吸油量が400ml/100g以上で、かつBET比表面積が1000m2/g以上のカーボンブラックがより好適に使用できる。DBP給油量は400〜1000ml/100gがより好ましく、400〜600ml/100gがさらに好ましい。このDBP吸油量が400ml/100gより小さく、かつBET比表面積が1000m2/gより小さい場合、またはDBP吸油量が400ml/100g、BET比表面積が1000m2/gのいずれかが前記数値より小さい場合には、所望の表面抵抗率と帯電圧半減衰時間を得るためにより多くの配合量が必要となり、結果的に導電性炭素材料の脱落が多くなりかつ流動性が低下する可能性がある。また、BET比表面積の上限については特に制限はないが、作業性を大きく損なわせる虞がある点で、1,500m2/g以下がより好ましい。 This conductive carbon black is not particularly limited by the raw material and the production method, but carbon black having a DBP oil absorption of 400 ml / 100 g or more and a BET specific surface area of 1000 m 2 / g or more can be used more suitably. . The DBP oil supply amount is more preferably 400 to 1000 ml / 100 g, further preferably 400 to 600 ml / 100 g. When the DBP oil absorption is smaller than 400 ml / 100 g and the BET specific surface area is smaller than 1000 m 2 / g, or when either the DBP oil absorption is 400 ml / 100 g or the BET specific surface area is 1000 m 2 / g smaller than the above value In order to obtain a desired surface resistivity and charged voltage half decay time, a larger amount of blending is required, and as a result, there is a possibility that the conductive carbon material is dropped and the fluidity is lowered. Moreover, there is no restriction | limiting in particular about the upper limit of a BET specific surface area, However, 1500 m < 2 > / g or less is more preferable at the point which may impair workability | operativity greatly.
ここでDBP吸油量とは、ジブチルフタレートアブソープトメーターによって測定された値で、導電性カーボンブラック100g当りに包含されるジブチルフタレートのml容量で、導電性カーボンブラックのストラクチャーの程度を示し、樹脂組成物に配合した際の導電性に影響するとされている。また、BET比表面積は液体窒素吸着法によって求めた値で、導電性カーボンブラック単位重量当たりの表面積を示す。 Here, the DBP oil absorption is a value measured by a dibutyl phthalate abstract meter, which is the ml capacity of dibutyl phthalate contained per 100 g of conductive carbon black, and indicates the degree of structure of the conductive carbon black. It is said to affect the conductivity when blended with the composition. Further, the BET specific surface area is a value obtained by a liquid nitrogen adsorption method and indicates the surface area per unit weight of the conductive carbon black.
(カーボンナノチューブ)
カーボンナノチューブとしては、特に原料、製法に制限されるものではないが、グラフェンシートの層数が1層、2層、または2層を超える複数層であってもよく、特に2層を超える複数層が好ましい。カーボンナノチューブの直径は0.7〜100nmが好ましく、7〜100nmがより好ましく、15〜90nmが更に好ましい。カーボンナノチューブのアスペクト比は5以上が好ましく、50以上がより好ましく、100以上が更に好ましい。
(carbon nanotube)
The carbon nanotube is not particularly limited by the raw material and the manufacturing method, but the number of graphene sheets may be one layer, two layers, or a plurality of layers exceeding two layers, particularly a plurality of layers exceeding two layers. Is preferred. The diameter of the carbon nanotube is preferably 0.7 to 100 nm, more preferably 7 to 100 nm, and still more preferably 15 to 90 nm. The aspect ratio of the carbon nanotube is preferably 5 or more, more preferably 50 or more, and still more preferably 100 or more.
アスペクト比は、走査型電子顕微鏡倍率3〜10万倍にて長さと直径を測定し、その比より求めることができる。なお、長さの測定は以下の方法で実施する。まずその観察像をCCDカメラに画像データとして取り込む。次に得られた画像データを、画像解析装置を使用して繊維長を算出する。測定本数は5000本以上として行う。また、直径の測定は以下の方法で実施する。まず電子顕微鏡の観察で得られる画像に対して、直径を測定する対象のカーボンナノチューブをランダムに抽出し、中央部に近いところで直径を測定する。なお、断面が円でない場合はその最大値を直径とする。得られた測定値から数平均直径を算出する。近年の電子顕微鏡はその観察画面上の長さを算出する機能が備えられているため、かかる直径も比較的容易に算出可能である。測定本数は1000本以上として行う。 The aspect ratio can be determined from the ratio of length and diameter measured at a scanning electron microscope magnification of 3 to 100,000. The length is measured by the following method. First, the observation image is taken into the CCD camera as image data. Next, the fiber length of the obtained image data is calculated using an image analyzer. The number of measurement is 5000 or more. The diameter is measured by the following method. First, carbon nanotubes whose diameter is to be measured are randomly extracted from an image obtained by observation with an electron microscope, and the diameter is measured near the center. If the cross section is not a circle, the maximum value is the diameter. The number average diameter is calculated from the measured values obtained. Since recent electron microscopes have a function of calculating the length on the observation screen, the diameter can be calculated relatively easily. The number of measurement is 1000 or more.
かかる導電性炭素材料(C成分)の含有量は、樹脂成分の合計100重量部に対し1〜20重量部であり、2〜15重量部が好ましく、3〜10重量部がより好ましい。導電性炭素材料の配合量が1重量部未満であれば、表面抵抗率と帯電圧減衰時間が本発明の請求範囲に入らず、導電性炭素材料の配合量が20重量部を超えると導電性炭素材料の脱落が多くなり好ましくない。 Content of this electroconductive carbon material (C component) is 1-20 weight part with respect to a total of 100 weight part of a resin component, 2-15 weight part is preferable and 3-10 weight part is more preferable. If the blending amount of the conductive carbon material is less than 1 part by weight, the surface resistivity and the charged voltage decay time do not fall within the scope of the present invention, and if the blending amount of the conductive carbon material exceeds 20 parts by weight, the conductivity is increased. It is not preferable because the carbon material is largely dropped.
<D成分:ガラス繊維及び/又はガラスフレーク>
本発明で使用されるガラス繊維及び/又はガラスフレークは、強度向上や成形品の反り低減のために配合する。
<D component: Glass fiber and / or glass flake>
The glass fiber and / or glass flake used in the present invention is blended for improving the strength and reducing the warpage of the molded product.
(ガラス繊維)
本発明で使用できるガラス繊維は、例えば長繊維タイプ(ロービング)や短繊維状のチョップドストランド、ミルドファイバーなどから選択して用いることができる。尚、ミルドファイバーにおいてはその数平均アスペクト比は5以上であることが好ましい。
(Glass fiber)
The glass fiber that can be used in the present invention can be selected from, for example, a long fiber type (roving), a short fiber chopped strand, a milled fiber, and the like. In the milled fiber, the number average aspect ratio is preferably 5 or more.
ガラス繊維は、集束剤(例えばポリ酢酸ビニル、ウレタン、アクリル、エポキシ、ポリエステル集束剤等)、カップリング剤(例えばアルキルアルコキシシランやポリオルガノハイドロジェンシロキサンなどを含むシラン化合物、ボロン化合物、チタン化合物等)、その他の表面処理剤で処理されていてもよい。かかるその他の表面処理剤としては、高級脂肪酸エステル、酸化合物(例えば、亜リン酸、リン酸、カルボン酸、およびカルボン酸無水物など)並びにワックスなどが例示される。さらに各種樹脂、高級脂肪酸エステル、およびワックスなどの集束剤で造粒し顆粒状とされていてもよい。 Glass fibers include sizing agents (for example, polyvinyl acetate, urethane, acrylic, epoxy, polyester sizing agents, etc.), coupling agents (for example, silane compounds, boron compounds, titanium compounds, etc. including alkylalkoxysilanes, polyorganohydrogensiloxanes, etc.) ) Or other surface treatment agents. Examples of such other surface treatment agents include higher fatty acid esters, acid compounds (for example, phosphorous acid, phosphoric acid, carboxylic acid, and carboxylic acid anhydride), and waxes. Furthermore, it may be granulated with a sizing agent such as various resins, higher fatty acid esters, and waxes.
(ガラスフレーク)
本発明に使用されるガラスフレークは、厚さに対して径が少なくとも数倍以上の鱗片状または層状の形状を有するもので、該導電性樹脂組成物からなる成形品の流動方向(MD)と垂直方向(TD)の成形収縮率の差を緩和、低減し、ソリの発生を低減するとともに寸法を安定させるために配合するものであるが、補助的に剛性の向上にも寄与する。ガラスフレークは、一般にその平均厚さと粒度の分布によって性状が表現され、これらの条件に特に限定されるものではないが、粒度については、標準ふるい法によるメジアン径が100〜500μmが好ましく、より好ましくは100〜400μm、更に好ましくは120〜300μm、特に好ましくは120〜200μmの範囲を挙げることができる。
(Glass flakes)
The glass flakes used in the present invention have a scaly or layered shape having a diameter of at least several times the thickness, and the flow direction (MD) of the molded product made of the conductive resin composition. It is blended to alleviate and reduce the difference in molding shrinkage in the vertical direction (TD), reduce warpage, and stabilize the dimensions, but also contributes to the improvement of rigidity. Glass flakes are generally expressed by their average thickness and particle size distribution, and are not particularly limited to these conditions, but for the particle size, the median diameter by the standard sieving method is preferably 100 to 500 μm, more preferably. May be in the range of 100 to 400 μm, more preferably 120 to 300 μm, and particularly preferably 120 to 200 μm.
本発明に使用されるガラスフレークは、従来公知の製造方法により得られる。例えば、溶融炉でガラス原料を溶融し、この融液をチューブ状に引き出し、ガラスの膜厚を一定にした後、ロールで粉砕することにより、特定の膜厚のフリットを得て、そのフリットを粉砕して所望のアスペクト比を有するフレークにすることができる。 The glass flakes used in the present invention can be obtained by a conventionally known production method. For example, a glass raw material is melted in a melting furnace, the melt is drawn into a tube shape, the glass film thickness is made constant, and then crushed with a roll to obtain a frit having a specific film thickness. It can be ground into flakes having the desired aspect ratio.
ここで、ガラスフレークの粒度をガラスフレークの厚さで除した値をガラスフレークのアスペクト比と定義すれば、このアスペクト比の値が好ましくは9以上(厚さ5μmの場合、粒度45μm以上)の粒度分布が合計で全体の75%以上のもの、さらに好ましくはアスペクト比の値が28以上(厚さ5μmの場合、粒度140μm以上)の粒度分布が合計で全体の80%以上のものが、当該導電性樹脂組成物からなる成形品の流動方向(MD)と垂直方向(TD)の収縮率の差を緩和、低減するうえで好適に使用できる。 Here, if the value obtained by dividing the particle size of the glass flake by the thickness of the glass flake is defined as the aspect ratio of the glass flake, the value of this aspect ratio is preferably 9 or more (when the thickness is 5 μm, the particle size is 45 μm or more). The total particle size distribution is 75% or more, more preferably the aspect ratio value is 28 or more (when the thickness is 5 μm, the particle size is 140 μm or more). It can be suitably used for reducing or reducing the difference in shrinkage between the flow direction (MD) and the vertical direction (TD) of a molded article made of a conductive resin composition.
かかるガラス繊維及び/又はガラスフレーク(D成分)は、A成分とB成分の合計100重量部当り5〜50重量部配合するのが好ましく、10〜40重量部がより好ましい。。ガラス繊維及び/又はガラスフレークを配合する場合は強度向上と成形品の反り低減が狙いであるが、5重量を下回ると所望の性能を得ることができず、50重量部を上回ると流動性が悪化し、生産性の面で好ましくない。もちろん、ガラス繊維とガラスフレークを所望の特性に応じて併用し、かつその配合比は所望の特性に応じて決めることは言うまでもない。 Such glass fiber and / or glass flake (component D) is preferably blended in an amount of 5 to 50 parts by weight, more preferably 10 to 40 parts by weight, per 100 parts by weight of the total of component A and component B. . When glass fibers and / or glass flakes are blended, the aim is to improve strength and reduce warpage of the molded product. However, if the amount is less than 5 parts by weight, the desired performance cannot be obtained. It deteriorates and is not preferable in terms of productivity. Of course, it goes without saying that glass fibers and glass flakes are used in combination according to the desired properties, and the blending ratio is determined according to the desired properties.
<E成分:ポリテトラフルオロエチレン粒子>
本発明で使用されるポリテトラフルオロエチレン粒子は、成形品に摺動性を付与し、導電性炭素材料の脱落を抑制するために配合する。
本発明のポリテトラフルオロエチレン粒子としては、低分子量ポリテトラフルオロエチレン、ポリビニリデンフルオライド、テトラフルオロエチレン・パーフルオロメチルビニルエーテル共重合体、テトラフルオロエチレン・ヘキサフルオロプロピレン共重合体、テトラフルオロエチレン・エチレン共重合体等が挙げられいずれの使用も可能であるが、中でも摺動性の面から低分子量ポリテトラフルオロエチレンの使用が好ましい。該低分子量ポリテトラフルオロエチレンには少量の共重合成分を含んでいるものも含まれる。低分子量ポリテトラフルオロエチレンとしては、通常乾性潤滑剤として使用されるものが使用でき、好ましくは、微粉末状である。微粉末の粒子径は、パークロルエチレン中に分散させた分散液を光透過法により測定する方法で平均0.1〜100μmのものが好ましい。またポリテトラフルオロエチレン微粉末の融点は、DSC法測定で320℃以上のものが好ましい。ポリテトラフルオロエチレン微粉末は再凝集しやすいので再凝集し難くするために焼成処理等の処理を施したものもあり、これらも好ましく使用できる。ポリテトラフルオロエチレン樹脂はダイキン工業(株)よりルブロンL−5,L−2,L−7として、また旭アイシーアイフロロポリマーズ(株)よりフルオンL−150J,L−169J,L−170J,L−172Jとして、また三井・デュポンフロロケミカル(株)よりTLP−10F−1として、またヘキストジャパン(株)よりホスタフロンTF9202,TF9205として市販されており、容易に入手可能である。
<E component: polytetrafluoroethylene particles>
The polytetrafluoroethylene particles used in the present invention are blended in order to impart slidability to the molded product and to prevent the conductive carbon material from falling off.
The polytetrafluoroethylene particles of the present invention include low molecular weight polytetrafluoroethylene, polyvinylidene fluoride, tetrafluoroethylene / perfluoromethyl vinyl ether copolymer, tetrafluoroethylene / hexafluoropropylene copolymer, tetrafluoroethylene / An ethylene copolymer or the like can be mentioned, and any of these can be used, but among them, the use of low molecular weight polytetrafluoroethylene is preferable from the viewpoint of slidability. The low molecular weight polytetrafluoroethylene includes those containing a small amount of a copolymer component. As the low molecular weight polytetrafluoroethylene, those usually used as dry lubricants can be used, and preferably in the form of fine powder. The average particle diameter of the fine powder is preferably 0.1 to 100 μm by a method of measuring a dispersion dispersed in perchlorethylene by a light transmission method. The melting point of the polytetrafluoroethylene fine powder is preferably 320 ° C. or higher as measured by DSC method. Since the polytetrafluoroethylene fine powder is easily re-agglomerated, some of it has been subjected to a treatment such as a baking treatment in order to make it difficult to re-agglomerate, and these can be preferably used. Polytetrafluoroethylene resin is Lubron L-5, L-2, L-7 from Daikin Industries, Ltd., and Fullon L-150J, L-169J, L-170J, L from Asahi IC Fluoropolymers Co., Ltd. It is commercially available as -172J, as TLP-10F-1 from Mitsui DuPont Fluorochemical Co., Ltd., and as Hostaflon TF9202 and TF9205 from Hoechst Japan Co., Ltd.
かかるポリテトラフルオロエチレン粒子は、A成分とB成分の合計100重量部当り1〜10重量部配合するのが好ましく、1〜5重量部がより好ましい。1重量を下回ると所望の摺動性を得られないために導電性炭素材料の脱落が抑制できず、10重量部を上回るとポリテトラフルオロエチレンの分散相が導電性炭素材料の導電経路を乱すため、成形品の表面抵抗率及び帯電圧半減衰時間に悪影響を及ぼす可能性がある。 Such polytetrafluoroethylene particles are preferably blended in an amount of 1 to 10 parts by weight, more preferably 1 to 5 parts by weight, per 100 parts by weight of the total of component A and component B. If the amount is less than 1 weight, the desired slidability cannot be obtained, so that the dropping of the conductive carbon material cannot be suppressed, and if the amount exceeds 10 parts by weight, the dispersed phase of polytetrafluoroethylene disturbs the conductive path of the conductive carbon material. Therefore, there is a possibility of adversely affecting the surface resistivity and the half voltage decay time of the molded product.
<F成分:酸化防止剤>
酸化防止剤(F成分)は、ホスファイト系化合物、ホスホナイト系化合物、ヒンダートフェノール系化合物およびチオエーテル系化合物からなる群より選ばれる少なくとも一種である。酸化防止剤(F成分)は、ホスファイト系化合物およびヒンダードフェノール系化合物の二種からなることが、熱安定性向上の面で特に好ましい。
<F component: Antioxidant>
The antioxidant (component F) is at least one selected from the group consisting of phosphite compounds, phosphonite compounds, hindered phenol compounds, and thioether compounds. The antioxidant (F component) is particularly preferably composed of two types of phosphite compounds and hindered phenol compounds in terms of improving thermal stability.
(ホスファイト系化合物)
ホスファイト系化合物として、トリフェニルホスファイト、トリス(ノニルフェニル)ホスファイト、トリデシルホスファイト、トリオクチルホスファイト、トリオクタデシルホスファイト、ジデシルモノフェニルホスファイト、ジオクチルモノフェニルホスファイト、ジイソプロピルモノフェニルホスファイト、モノブチルジフェニルホスファイト、モノデシルジフェニルホスファイト、モノオクチルジフェニルホスファイト、トリス(ジエチルフェニル)ホスファイト、トリス(ジ−iso−プロピルフェニル)ホスファイト、トリス(ジ−n−ブチルフェニル)ホスファイト、トリス(2,4−ジ−tert−ブチルフェニル)ホスファイト、トリス(2,6−ジ−tert−ブチルフェニル)ホスファイト、ジステアリルペンタエリスリトールジホスファイト、ビス(2,4−ジ−tert−ブチルフェニル)ペンタエリスリトールジホスファイト、ビス(2,6−ジ−tert−ブチル−4−メチルフェニル)ペンタエリスリトールジホスファイト、ビス(2,6−ジ−tert−ブチル−4−エチルフェニル)ペンタエリスリトールジホスファイト、ビス{2,4−ビス(1−メチル−1−フェニルエチル)フェニル}ペンタエリスリトールジホスファイト、フェニルビスフェノールAペンタエリスリトールジホスファイト、ビス(ノニルフェニル)ペンタエリスリトールジホスファイト、およびジシクロヘキシルペンタエリスリトールジホスファイト等が挙げられる。
(Phosphite compounds)
As phosphite compounds, triphenyl phosphite, tris (nonylphenyl) phosphite, tridecyl phosphite, trioctyl phosphite, trioctadecyl phosphite, didecyl monophenyl phosphite, dioctyl monophenyl phosphite, diisopropyl monophenyl Phosphite, monobutyl diphenyl phosphite, monodecyl diphenyl phosphite, monooctyl diphenyl phosphite, tris (diethylphenyl) phosphite, tris (di-iso-propylphenyl) phosphite, tris (di-n-butylphenyl) Phosphite, tris (2,4-di-tert-butylphenyl) phosphite, tris (2,6-di-tert-butylphenyl) phosphite, distearyl pentaeri Ritol diphosphite, bis (2,4-di-tert-butylphenyl) pentaerythritol diphosphite, bis (2,6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphite, bis ( 2,6-di-tert-butyl-4-ethylphenyl) pentaerythritol diphosphite, bis {2,4-bis (1-methyl-1-phenylethyl) phenyl} pentaerythritol diphosphite, phenylbisphenol A penta Examples include erythritol diphosphite, bis (nonylphenyl) pentaerythritol diphosphite, and dicyclohexyl pentaerythritol diphosphite.
さらに他のホスファイト系化合物としては二価フェノール類と反応し環状構造を有するものも使用できる。例えば、2,2’−メチレンビス(4,6−ジ−tert−ブチルフェニル)(2,4−ジ−tert−ブチルフェニル)ホスファイト、2,2’−メチレンビス(4,6−ジ−tert−ブチルフェニル)(2−tert−ブチル−4−メチルフェニル)ホスファイト、および2,2−メチレンビス(4,6−ジ−tert−ブチルフェニル)オクチルホスファイト等が挙げられる。 Furthermore, as other phosphite compounds, those that react with dihydric phenols and have a cyclic structure can be used. For example, 2,2′-methylenebis (4,6-di-tert-butylphenyl) (2,4-di-tert-butylphenyl) phosphite, 2,2′-methylenebis (4,6-di-tert- Butylphenyl) (2-tert-butyl-4-methylphenyl) phosphite, 2,2-methylenebis (4,6-di-tert-butylphenyl) octyl phosphite, and the like.
好適なホスファイト系化合物は、ジステアリルペンタエリスリトールジホスファイト、ビス(2,4−ジ−tert−ブチルフェニル)ペンタエリスリトールジホスファイト、ビス(2,6−ジ−tert−ブチル−4−メチルフェニル)ペンタエリスリトールジホスファイト、およびビス{2,4−ビス(1−メチル−1−フェニルエチル)フェニル}ペンタエリスリトールジホスファイトである。 Suitable phosphite compounds are distearyl pentaerythritol diphosphite, bis (2,4-di-tert-butylphenyl) pentaerythritol diphosphite, bis (2,6-di-tert-butyl-4-methyl). Phenyl) pentaerythritol diphosphite, and bis {2,4-bis (1-methyl-1-phenylethyl) phenyl} pentaerythritol diphosphite.
(ホスホナイト系化合物)
ホスホナイト化合物として、テトラキス(2,4−ジ−tert−ブチルフェニル)−4,4’−ビフェニレンジホスホナイト、テトラキス(2,4−ジ−tert−ブチルフェニル)−4,3’−ビフェニレンジホスホナイト、テトラキス(2,4−ジ−tert−ブチルフェニル)−3,3’−ビフェニレンジホスホナイト、テトラキス(2,6−ジ−tert−ブチルフェニル)−4,4’−ビフェニレンジホスホナイト、テトラキス(2,6−ジ−tert−ブチルフェニル)−4,3’−ビフェニレンジホスホナイト、テトラキス(2,6−ジ−tert−ブチルフェニル)−3,3’−ビフェニレンジホスホナイト、ビス(2,4−ジ−tert−ブチルフェニル)−4−フェニル−フェニルホスホナイト、ビス(2,4−ジ−tert−ブチルフェニル)−3−フェニル−フェニルホスホナイト、ビス(2,6−ジ−n−ブチルフェニル)−3−フェニル−フェニルホスホナイト、ビス(2,6−ジ−tert−ブチルフェニル)−4−フェニル−フェニルホスホナイト、ビス(2,6−ジ−tert−ブチルフェニル)−3−フェニル−フェニルホスホナイト等が挙げられる。テトラキス(ジ−tert−ブチルフェニル)−ビフェニレンジホスホナイト、ビス(ジ−tert−ブチルフェニル)−フェニル−フェニルホスホナイトが好ましく、テトラキス(2,4−ジ−tert−ブチルフェニル)−ビフェニレンジホスホナイト、ビス(2,4−ジ−tert−ブチルフェニル)−フェニル−フェニルホスホナイトがより好ましい。かかるホスホナイト化合物は上記アルキル基が2以上置換したアリール基を有するホスファイト化合物との併用可能であり好ましい。
(Phosphonite compounds)
Examples of phosphonite compounds include tetrakis (2,4-di-tert-butylphenyl) -4,4′-biphenylene diphosphonite, tetrakis (2,4-di-tert-butylphenyl) -4,3′-biphenylene diphospho. Knight, tetrakis (2,4-di-tert-butylphenyl) -3,3'-biphenylenediphosphonite, tetrakis (2,6-di-tert-butylphenyl) -4,4'-biphenylenediphosphonite, Tetrakis (2,6-di-tert-butylphenyl) -4,3′-biphenylenediphosphonite, tetrakis (2,6-di-tert-butylphenyl) -3,3′-biphenylenediphosphonite, bis ( 2,4-di-tert-butylphenyl) -4-phenyl-phenylphosphonite, bis (2,4-di-tert Butylphenyl) -3-phenyl-phenylphosphonite, bis (2,6-di-n-butylphenyl) -3-phenyl-phenylphosphonite, bis (2,6-di-tert-butylphenyl) -4- Examples thereof include phenyl-phenylphosphonite, bis (2,6-di-tert-butylphenyl) -3-phenyl-phenylphosphonite. Tetrakis (di-tert-butylphenyl) -biphenylene diphosphonite, bis (di-tert-butylphenyl) -phenyl-phenylphosphonite are preferred, and tetrakis (2,4-di-tert-butylphenyl) -biphenylene diphospho Knight and bis (2,4-di-tert-butylphenyl) -phenyl-phenylphosphonite are more preferred. Such a phosphonite compound is preferable because it can be used in combination with a phosphite compound having an aryl group in which two or more alkyl groups are substituted.
ホスホナイト化合物としてはテトラキス(2,4−ジ−tert−ブチルフェニル)−ビフェニレンジホスホナイトが好ましく、該ホスホナイトを主成分とする安定剤は、Sandostab P−EPQ(商標、Clariant社製)およびIrgafos P−EPQ(商標、CIBA SPECIALTY CHEMICALS社製)として市販されておりいずれも利用できる。 The phosphonite compound is preferably tetrakis (2,4-di-tert-butylphenyl) -biphenylenediphosphonite, and stabilizers based on the phosphonite are Sandostab P-EPQ (trademark, manufactured by Clariant) and Irgafos P. -It is commercially available as EPQ (trademark, manufactured by CIBA SPECIALTY CHEMICALS) and any of them can be used.
(ヒンダードフェノール系化合物)
ヒンダードフェノール化合物としては、通常樹脂に配合される各種の化合物が使用できる。かかるヒンダードフェノール化合物としては、α−トコフェロール、ブチルヒドロキシトルエン、シナピルアルコール、ビタミンE、オクタデシル−3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート、2−tert−ブチル−6−(3’−tert−ブチル−5’−メチル−2’−ヒドロキシベンジル)−4−メチルフェニルアクリレート、2,6−ジ−tert−ブチル−4−(N,N−ジメチルアミノメチル)フェノール、3,5−ジ−tert−ブチル−4−ヒドロキシベンジルホスホネートジエチルエステル、2,2’−メチレンビス(4−メチル−6−tert−ブチルフェノール)、2,2’−メチレンビス(4−エチル−6−tert−ブチルフェノール)、4,4’−メチレンビス(2,6−ジ−tert−ブチルフェノール)、2,2’−メチレンビス(4−メチル−6−シクロヘキシルフェノール)、2,2’−ジメチレン−ビス(6−α−メチル−ベンジル−p−クレゾール)、2,2’−エチリデン−ビス(4,6−ジ−tert−ブチルフェノール)、2,2’−ブチリデン−ビス(4−メチル−6−tert−ブチルフェノール)、4,4’−ブチリデンビス(3−メチル−6−tert−ブチルフェノール)、トリエチレングリコール−N−ビス−3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオネート、1,6−へキサンジオールビス[3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート]、ビス[2−tert−ブチル−4−メチル−6−(3−tert−ブチル−5−メチル−2−ヒドロキシベンジル)フェニル]テレフタレート、3,9−ビス{2−[3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオニルオキシ]−1,1,−ジメチルエチル}−2,4,8,10−テトラオキサスピロ[5,5]ウンデカン、4,4’−チオビス(6−tert−ブチル−m−クレゾール)、4,4’−チオビス(3−メチル−6−tert−ブチルフェノール)、2,2’−チオビス(4−メチル−6−tert−ブチルフェノール)、ビス(3,5−ジ−tert−ブチル−4−ヒドロキシベンジル)スルフィド、4,4’−ジ−チオビス(2,6−ジ−tert−ブチルフェノール)、4,4’−トリ−チオビス(2,6−ジ−tert−ブチルフェノール)、2,2−チオジエチレンビス−[3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート]、2,4−ビス(n−オクチルチオ)−6−(4−ヒドロキシ−3,5−ジ−tert−ブチルアニリノ)−1,3,5−トリアジン、N,N’−ヘキサメチレンビス−(3,5−ジ−tert−ブチル−4−ヒドロキシヒドロシンナミド)、N,N’−ビス[3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオニル]ヒドラジン、1,1,3−トリス(2−メチル−4−ヒドロキシ−5−tert−ブチルフェニル)ブタン、1,3,5−トリメチル−2,4,6−トリス(3,5−ジ−tert−ブチル−4−ヒドロキシベンジル)ベンゼン、トリス(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)イソシアヌレート、トリス(3,5−ジ−tert−ブチル−4−ヒドロキシベンジル)イソシアヌレート、1,3,5−トリス(4−tert−ブチル−3−ヒドロキシ−2,6−ジメチルベンジル)イソシアヌレート、1,3,5−トリス2[3(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオニルオキシ]エチルイソシアヌレート、テトラキス[メチレン−3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート]メタン、トリエチレングリコール−N−ビス−3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオネート、トリエチレングリコール−N−ビス−3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)アセテート、3,9−ビス[2−{3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)アセチルオキシ}−1,1−ジメチルエチル]−2,4,8,10−テトラオキサスピロ[5,5]ウンデカン、テトラキス[メチレン−3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオネート]メタン、1,3,5−トリメチル−2,4,6−トリス(3−tert−ブチル−4−ヒドロキシ−5−メチルベンジル)ベンゼン、およびトリス(3−tert−ブチル−4−ヒドロキシ−5−メチルベンジル)イソシアヌレート等が例示される。
(Hindered phenolic compounds)
As the hindered phenol compound, various compounds usually blended in a resin can be used. Examples of such hindered phenol compounds include α-tocopherol, butylhydroxytoluene, sinapyl alcohol, vitamin E, octadecyl-3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate, 2-tert-butyl. -6- (3'-tert-butyl-5'-methyl-2'-hydroxybenzyl) -4-methylphenyl acrylate, 2,6-di-tert-butyl-4- (N, N-dimethylaminomethyl) Phenol, 3,5-di-tert-butyl-4-hydroxybenzylphosphonate diethyl ester, 2,2′-methylenebis (4-methyl-6-tert-butylphenol), 2,2′-methylenebis (4-ethyl-6) -Tert-butylphenol), 4,4'-methylenebis (2,6-di-t) rt-butylphenol), 2,2′-methylenebis (4-methyl-6-cyclohexylphenol), 2,2′-dimethylene-bis (6-α-methyl-benzyl-p-cresol), 2,2′-ethylidene -Bis (4,6-di-tert-butylphenol), 2,2'-butylidene-bis (4-methyl-6-tert-butylphenol), 4,4'-butylidenebis (3-methyl-6-tert-butylphenol) ), Triethylene glycol-N-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, 1,6-hexanediol bis [3- (3,5-di-tert- Butyl-4-hydroxyphenyl) propionate], bis [2-tert-butyl-4-methyl-6- (3-tert-butyl- -Methyl-2-hydroxybenzyl) phenyl] terephthalate, 3,9-bis {2- [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionyloxy] -1,1, -dimethylethyl } -2,4,8,10-tetraoxaspiro [5,5] undecane, 4,4′-thiobis (6-tert-butyl-m-cresol), 4,4′-thiobis (3-methyl-6) -Tert-butylphenol), 2,2'-thiobis (4-methyl-6-tert-butylphenol), bis (3,5-di-tert-butyl-4-hydroxybenzyl) sulfide, 4,4'-di- Thiobis (2,6-di-tert-butylphenol), 4,4′-tri-thiobis (2,6-di-tert-butylphenol), 2,2-thiodiethylene S- [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], 2,4-bis (n-octylthio) -6- (4-hydroxy-3,5-di-tert- Butylanilino) -1,3,5-triazine, N, N′-hexamethylenebis- (3,5-di-tert-butyl-4-hydroxyhydrocinnamide), N, N′-bis [3- (3 , 5-Di-tert-butyl-4-hydroxyphenyl) propionyl] hydrazine, 1,1,3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, 1,3,5-trimethyl -2,4,6-tris (3,5-di-tert-butyl-4-hydroxybenzyl) benzene, tris (3,5-di-tert-butyl-4-hydroxyphenyl) isocyanur Rate, tris (3,5-di-tert-butyl-4-hydroxybenzyl) isocyanurate, 1,3,5-tris (4-tert-butyl-3-hydroxy-2,6-dimethylbenzyl) isocyanurate, 1,3,5-tris2 [3 (3,5-di-tert-butyl-4-hydroxyphenyl) propionyloxy] ethyl isocyanurate, tetrakis [methylene-3- (3,5-di-tert-butyl- 4-hydroxyphenyl) propionate] methane, triethylene glycol-N-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, triethylene glycol-N-bis-3- (3- tert-butyl-4-hydroxy-5-methylphenyl) acetate, 3,9-bis [2- {3 (3-tert-butyl-4-hydroxy-5-methylphenyl) acetyloxy} -1,1-dimethylethyl] -2,4,8,10-tetraoxaspiro [5,5] undecane, tetrakis [methylene- 3- (3-tert-Butyl-4-hydroxy-5-methylphenyl) propionate] methane, 1,3,5-trimethyl-2,4,6-tris (3-tert-butyl-4-hydroxy-5- Examples include methylbenzyl) benzene and tris (3-tert-butyl-4-hydroxy-5-methylbenzyl) isocyanurate.
上記化合物の中でも、本発明においてはテトラキス[メチレン−3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオネート]メタン、オクタデシル−3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート、および3,9−ビス[2−{3−(3−t−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオニルオキシ}−1,1−ジメチルエチル]−2,4,8,10−テトラオキサスピロ[5,5]ウンデカンが好ましく利用される。特に3,9−ビス[2−{3−(3−t−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオニルオキシ}−1,1−ジメチルエチル]−2,4,8,10−テトラオキサスピロ[5,5]ウンデカンが好ましい。上記ヒンダードフェノール系化合物は、単独でまたは2種以上を組合せて使用することができる。 Among the above compounds, tetrakis [methylene-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate] methane, octadecyl-3- (3,5-di-tert-butyl-) is used in the present invention. 4-hydroxyphenyl) propionate, and 3,9-bis [2- {3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionyloxy} -1,1-dimethylethyl] -2,4 , 8,10-Tetraoxaspiro [5,5] undecane is preferably used. In particular, 3,9-bis [2- {3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionyloxy} -1,1-dimethylethyl] -2,4,8,10-tetraoxa Spiro [5,5] undecane is preferred. The said hindered phenol type compound can be used individually or in combination of 2 or more types.
(チオエーテル系化合物)
チオエーテル系化合物の具体例として、ジラウリルチオジプロピオネート、ジトリデシルチオジプロピオネート、ジミリスチルチオジプロピオネート、ジステアリルチオジプロピオネート、ペンタエリスリトール−テトラキス(3−ラウリルチオプロピオネート)、ペンタエリスリトール−テトラキス(3−ドデシルチオプロピオネート)、ペンタエリスリトール−テトラキス(3−オクタデシルチオプロピオネート)、ペンタエリスリトールテトラキス(3−ミリスチルチオプロピオネート)、ペンタエリスリトール−テトラキス(3−ステアリルチオプロピオネート)等が挙げられる。
(Thioether compounds)
Specific examples of thioether compounds include dilauryl thiodipropionate, ditridecyl thiodipropionate, dimyristyl thiodipropionate, distearyl thiodipropionate, pentaerythritol-tetrakis (3-lauryl thiopropionate), Pentaerythritol-tetrakis (3-dodecylthiopropionate), pentaerythritol-tetrakis (3-octadecylthiopropionate), pentaerythritol tetrakis (3-myristylthiopropionate), pentaerythritol-tetrakis (3-stearylthio) Propionate) and the like.
かかる酸化防止剤(F成分)の含有量は、A成分とB成分の合計100重量部当たり、0.001〜2重量部が好ましく、より好ましくは0.005〜1重量部、さらに好ましくは0.01〜0.5重量部である。かかる配合量が0.001重量部より少ない場合は酸化防止効果が不足するため滞留熱安定性が低下し、2重量部を超えると、かえって酸化防止効果が低下するばかりか、酸化防止剤由来の揮発分による発生ガス量が多くなり、成形品のクリーン性を損ねる可能性がある。 The content of such an antioxidant (component F) is preferably 0.001 to 2 parts by weight, more preferably 0.005 to 1 part by weight, and still more preferably 0 per 100 parts by weight of the total of component A and component B. 0.01 to 0.5 parts by weight. When the blending amount is less than 0.001 part by weight, the anti-oxidation effect is insufficient, so the residence heat stability is lowered. When it exceeds 2 parts by weight, not only the antioxidant effect is lowered, but also the antioxidant-derived effect is derived. The amount of gas generated due to volatile matter increases, and the cleanliness of the molded product may be impaired.
また、前記リン系安定剤とヒンダードフェノール系安定剤を組み合わせて使用することが好ましい。リン系安定剤とヒンダードフェノール系安定剤を組み合わせて使用することで、安定剤としての相乗効果が発揮され、より成形時の熱安定性悪化を抑制できる。 Moreover, it is preferable to use the phosphorus stabilizer and the hindered phenol stabilizer in combination. By using a combination of a phosphorus-based stabilizer and a hindered phenol-based stabilizer, a synergistic effect as a stabilizer is exhibited, and deterioration of thermal stability during molding can be further suppressed.
<その他の添加剤>
本発明の組成物には、本発明の効果を発揮する範囲で、他の熱可塑性樹脂(例えば、ポリアリレート樹脂、液晶性ポリエステル樹脂、ポリアミド樹脂、ポリイミド樹脂、ポリエーテルイミド樹脂、ポリウレタン樹脂、シリコーン樹脂、ポリフェニレンエーテル、ポリフェニレンスルフィド樹脂、ポリスルホン樹脂、ポリエチレンおよびポリプロピレンなどのポリオレフィン樹脂、ポリスチレン樹脂、アクリロニトリル/スチレン共重合体(AS樹脂)、アクリロニトリル/ブタジエン/スチレン共重合体(ABS樹脂)、ポリスチレン樹脂、高衝撃ポリスチレン樹脂、シンジオタクチックポリスチレン樹脂、ポリメタクリレート樹脂、並びにフェノキシまたはエポキシ樹脂など)、D成分を除く無機充填剤(炭素繊維、炭素フレークなど)、有機充填剤(アラミド繊維、ケナフ繊維など)、衝撃改質剤(コアシェル型アクリルゴム、コアシェル型ブタジエンゴムなど)、紫外線吸収剤(ベンゾトリアゾール系、トリアジン系、ベンゾフェノン系など)、光安定剤(HALSなど)、離型剤(飽和脂肪酸エステル、不飽和脂肪酸エステル、パラフィンワックス、蜜蝋など)、流動改質剤(ポリカプロラクトンなど)、着色剤(カーボンブラック、二酸チタン、各種の有機染料、メタリック顔料など)、帯電防止剤、無機および有機の抗菌剤、光触媒系防汚剤(微粒子酸化チタン、微粒子酸化亜鉛など)、赤外線吸収剤、並びにフォトクロミック剤紫外線吸収剤などを配合してもよい。これら各種の添加剤は、周知の配合量で利用することができる。
<Other additives>
In the composition of the present invention, other thermoplastic resins (for example, polyarylate resin, liquid crystalline polyester resin, polyamide resin, polyimide resin, polyetherimide resin, polyurethane resin, silicone) Resin, polyphenylene ether, polyphenylene sulfide resin, polysulfone resin, polyolefin resin such as polyethylene and polypropylene, polystyrene resin, acrylonitrile / styrene copolymer (AS resin), acrylonitrile / butadiene / styrene copolymer (ABS resin), polystyrene resin, High impact polystyrene resin, syndiotactic polystyrene resin, polymethacrylate resin, phenoxy or epoxy resin, etc.), inorganic filler excluding D component (carbon fiber, carbon flake, etc.), Machine fillers (aramid fibers, kenaf fibers, etc.), impact modifiers (core shell acrylic rubber, core shell butadiene rubber, etc.), UV absorbers (benzotriazole, triazine, benzophenone, etc.), light stabilizers (HALS) ), Mold release agents (saturated fatty acid esters, unsaturated fatty acid esters, paraffin wax, beeswax, etc.), flow modifiers (polycaprolactone, etc.), colorants (carbon black, titanium diacid, various organic dyes, metallic pigments) Etc.), antistatic agents, inorganic and organic antibacterial agents, photocatalytic antifouling agents (fine particle titanium oxide, fine particle zinc oxide, etc.), infrared absorbers, photochromic agents and ultraviolet absorbers. These various additives can be used in known amounts.
<導電性樹脂組成物の製造>
本発明の導電性樹脂組成物の製造には、任意の方法が採用される。例えばA成分からF成分を、V型ブレンダー、ヘンシェルミキサー、メカノケミカル装置、および押出混合機などの予備混合手段を用いて充分に混合(いわゆるドライブレンド)した後、必要に応じて押出造粒器やブリケッティングマシーンなどにより得られた予備混合物の造粒を行い、その後ベント式二軸押出機に代表される溶融混練機で溶融混練し、溶融混練後の組成物をペレタイザー等の機器によりペレット化する方法が挙げられる。
<Manufacture of conductive resin composition>
Arbitrary methods are employ | adopted for manufacture of the conductive resin composition of this invention. For example, components A to F are sufficiently mixed (so-called dry blend) using premixing means such as a V-type blender, a Henschel mixer, a mechanochemical apparatus, and an extrusion mixer, and then an extrusion granulator as necessary. Granulation of the pre-mixture obtained by using a briquetting machine, etc., and then melt-kneading with a melt-kneader typified by a vent type twin-screw extruder, and pelletizing the melt-kneaded composition with a device such as a pelletizer The method of making it.
他に、各成分をそれぞれ独立にベント式二軸押出機に代表される溶融混練機に供給する方法や、各成分の一部を予備混合した後、残りの成分と独立に溶融混練機に供給する方法なども挙げられる。予備混合する方法としては例えば、A成分のパウダーの一部とD成分及びD成分などの配合する添加剤とをドライブレンドして、パウダーで希釈された添加剤のマスターバッチを作成する方法が挙げられる。更に一成分を独立に溶融押出機の途中から供給する方法なども挙げられる。これら溶融混練に際しての加熱温度は、通常250〜300℃の範囲で選ばれる。 In addition, a method of supplying each component independently to a melt kneader represented by a vent type twin screw extruder, or a part of each component is premixed and then supplied to the melt kneader independently of the remaining components. The method of doing is also mentioned. Examples of the premixing method include a method of dry blending a part of the powder of the A component and the additive such as the D component and the D component to prepare a master batch of the additive diluted with the powder. It is done. Furthermore, the method etc. which supply one component independently from the middle of a melt extruder are mentioned. The heating temperature at the time of melt kneading is usually selected in the range of 250 to 300 ° C.
尚、配合する成分に液状のものがある場合には、溶融押出機への供給にいわゆる液注装置、または液添装置を使用することができる。かかる液注装置、または液添装置は加温装置が設置されているものが好ましく使用される。 In addition, when there exists a liquid thing in the component to mix | blend, what is called a liquid injection apparatus or a liquid addition apparatus can be used for supply to a melt extruder. As such a liquid injection device or a liquid addition device, one provided with a heating device is preferably used.
押出された樹脂は、直接切断してペレット化するか、またはストランドを形成した後かかるストランドをペレタイザーで切断してペレット化することができる。ペレット化に際して外部の埃などの影響を低減する必要がある場合には、押出機周囲の雰囲気を清浄化することが好ましい。得られたペレットの形状は、円柱、角柱、および球状など一般的な形状を取り得るが、より好適には円柱である。かかる円柱の直径は好ましくは1〜5mm、より好ましくは1.5〜4mm、さらに好ましくは2〜3.3mmである。一方、円柱の長さは好ましくは1〜30mm、より好ましくは2〜5mm、さらに好ましくは2.5〜3.5mmである。 The extruded resin can be cut directly into pellets or formed into strands and then cut into pellets with a pelletizer. When it is necessary to reduce the influence of external dust during pelletization, it is preferable to clean the atmosphere around the extruder. Although the shape of the obtained pellet can take general shapes, such as a cylinder, a prism, and a spherical shape, it is more preferably a cylinder. The diameter of such a cylinder is preferably 1 to 5 mm, more preferably 1.5 to 4 mm, and still more preferably 2 to 3.3 mm. On the other hand, the length of the cylinder is preferably 1 to 30 mm, more preferably 2 to 5 mm, and still more preferably 2.5 to 3.5 mm.
本発明の樹脂組成物は、発生ガス量が2ppm以下であるものが好ましく、1ppm以下であるものがより好ましく、更には0.5ppm以下であるものがより好ましい。かかる発生ガス量が2ppmを超えると、クリーン性が悪化し、成形品周辺の精密部品に影響を及ぼす可能性があるため、好ましくない。なお樹脂組成物の発生ガス量は下記の方法で測定した。すなわち、本発明の導電性樹脂組成物ペレットをガスクロマトグラム(アジレント社製 GC‐MS)を使用し揮発性有機ガス量を測定した。具体的には、押出した組成物ペレット3gを150℃にて1時間加熱し、ガスクロマトグラム(GC−MS)にて揮発性有機ガス量を測定し、その総量をトルエン換算したものを発生ガス量とした。 The resin composition of the present invention preferably has a generated gas amount of 2 ppm or less, more preferably 1 ppm or less, and even more preferably 0.5 ppm or less. If the amount of generated gas exceeds 2 ppm, the cleanliness deteriorates and there is a possibility of affecting the precision parts around the molded product, which is not preferable. The generated gas amount of the resin composition was measured by the following method. That is, the amount of volatile organic gas was measured for the conductive resin composition pellets of the present invention using a gas chromatogram (GC-MS manufactured by Agilent). Specifically, 3 g of the extruded composition pellets was heated at 150 ° C. for 1 hour, the amount of volatile organic gas was measured with a gas chromatogram (GC-MS), and the total amount was converted to toluene, and the amount of gas generated It was.
<成形品の作成>
本発明の導電性樹脂組成物からなる成形品は、通常上記の如く製造されたペレットを射出成形して成形品を得ることにより各種製品を製造することができる。かかる射出成形においては、通常の成形方法だけでなく、射出圧縮成形、射出プレス成形、ガスアシスト射出成形、発泡成形(超臨界流体を注入する方法を含む)、インサート成形、インモールドコーティング成形、断熱金型成形、急速加熱冷却金型成形、二色成形、サンドイッチ成形、および超高速射出成形などを挙げることができる。また成形はコールドランナー方式およびホットランナー方式のいずれも選択することができる。射出成形品は、従来公知の成形法が何ら限定なく適用できるが、射出成形時、外観を上げる観点から、金型温度は好ましくは30℃以上、より好ましくは40℃以上である。しかし、成形品の変形を防ぐ意味において、金型温度は、好ましくは100℃以下、さらに好ましくは90℃以下である。また本発明の導電性樹脂組成物からなる成形品は、押出成形、回転成形やブロー成形などにより得ることも可能である。
<Creation of molded products>
Various products can be produced from the molded product comprising the conductive resin composition of the present invention by obtaining a molded product by injection molding the pellets produced as described above. In such injection molding, not only ordinary molding methods but also injection compression molding, injection press molding, gas assist injection molding, foam molding (including a method of injecting a supercritical fluid), insert molding, in-mold coating molding, heat insulation Examples thereof include mold molding, rapid heating / cooling mold molding, two-color molding, sandwich molding, and ultra-high speed injection molding. In addition, either a cold runner method or a hot runner method can be selected for molding. Conventionally known molding methods can be applied to the injection-molded product without any limitation, but the mold temperature is preferably 30 ° C. or higher, more preferably 40 ° C. or higher from the viewpoint of improving the appearance during injection molding. However, the mold temperature is preferably 100 ° C. or lower, more preferably 90 ° C. or lower in the sense of preventing the deformation of the molded product. Moreover, the molded article which consists of the conductive resin composition of this invention can also be obtained by extrusion molding, rotational molding, blow molding, etc.
さらに本発明の導電性樹脂組成物からなる成形品は、表面改質を施すことによりさらに他の機能を付与することが可能である。ここでいう表面改質とは、蒸着(物理蒸着、化学蒸着等)、メッキ(電気メッキ、無電解メッキ、溶融メッキ等)、塗装、コーティング、印刷等の樹脂成形品の表層上に新たな層を形成させるものであり、通常の樹脂成形品に用いられる方法が適用できる。 Furthermore, the molded article made of the conductive resin composition of the present invention can be imparted with other functions by surface modification. Surface modification here means a new layer on the surface of resin molded products such as vapor deposition (physical vapor deposition, chemical vapor deposition, etc.), plating (electroplating, electroless plating, hot dipping, etc.), painting, coating, printing, etc. The method used for normal resin molded products can be applied.
本発明の導電性樹脂組成物からなる成形品の用途としては、ハードディスク関連部品およびその工程内容器、ICチップトレイ、ウェハー搬送容器、ガラスコンテナ、並びに自動車外装部品が挙げられる。 Applications of the molded article comprising the conductive resin composition of the present invention include hard disk related parts and their in-process containers, IC chip trays, wafer transfer containers, glass containers, and automobile exterior parts.
本発明の成形品の表面抵抗率は105〜1012Ω/sqであり、106〜1010Ω/sqが好ましく、107〜109Ω/sqがより好ましい。かかる表面抵抗率が105Ω/sqより低いと電荷が近づいてきた際のスパークがより起こりやすくなるため好ましくない。一方、1012Ω/sqより高いと電荷が帯電しやすく、スパーク電流が大きくなるため好ましくない。なお、成形品の表面抵抗率の測定はそれぞれの抵抗値に合った抵抗率計を使用して測定した。すなわち、1010Ω/sq以上の場合は、TOA株式会社製 デジタル絶縁計DSM-8103(印加電圧100V、専用プローブ)、107〜1010Ω/sqの場合には、三菱化学株式会社製 ハイレスターUP MCP-HT400(印加電圧100V、UR-SSプローブ(JISK6911準拠))、107Ω/sq以下の場合には、三菱化学株式会社製 ロレスターGP MCP-T600(印加電圧90V、ESPプローブ(JISK7194準拠))を使用した。具体的な測定方法としては、成形品から試験片(縦×横×厚み=90mm×50mm×2mmt)を3個切削し、温度23℃、湿度50%RHの条件下において前記の抵抗率計を使用して試験片面内の中央部の表面抵抗率を測定し3個の試験片から得られた値の平均値を試験片の表面抵抗率とした。 The surface resistivity of the molded product of the present invention is 10 5 to 10 12 Ω / sq, preferably 10 6 to 10 10 Ω / sq, and more preferably 10 7 to 10 9 Ω / sq. When the surface resistivity is lower than 10 5 Ω / sq, it is not preferable because spark when the electric charge approaches is more likely to occur. On the other hand, if it is higher than 10 12 Ω / sq, the electric charge is easily charged and the spark current becomes large, which is not preferable. The surface resistivity of the molded product was measured using a resistivity meter suitable for each resistance value. That is, in the case of 10 10 Ω / sq or more, digital insulation meter DSM-8103 (applied voltage 100 V, dedicated probe) manufactured by TOA Co., Ltd., and in the case of 10 7 to 10 10 Ω / sq, manufactured by Mitsubishi Chemical Corporation High Lester UP MCP-HT400 (applied voltage 100V, UR-SS probe (JISK6911 compliant)), 10 7 Ω / sq or less, Lorester GP MCP-T600 (applied voltage 90V, ESP probe (JISK7194) Compliant)). As a specific measurement method, three test pieces (length × width × thickness = 90 mm × 50 mm × 2 mmt) are cut from the molded product, and the above-described resistivity meter is used under the conditions of a temperature of 23 ° C. and a humidity of 50% RH. The surface resistivity of the central part in the test piece surface was measured and the average value of the values obtained from the three test pieces was defined as the surface resistivity of the test piece.
なお、本発明の成形品における表面抵抗率は、樹脂組成物の流動性に大きく影響を受けるため、その調整方法の一つに流動性を制御する方法を取ることができる。具体的には、樹脂組成物のメルトボリュームフローレイト(MVR)は、好ましくは2〜80cm3/10分、より好ましくは3〜50cm3/10分、更により好ましくは5〜20cm3/10分を示すとき、良好な表面抵抗率を得ることができる。かかる樹脂組成物のメルトボリュームフローレイトは、ISO1133(JIS K 7210)に準拠する方法で、シリンダー及びピストン温度を300℃、荷重1.2kgにて測定する。 In addition, since the surface resistivity in the molded article of the present invention is greatly influenced by the fluidity of the resin composition, a method of controlling the fluidity can be taken as one of the adjustment methods. Specifically, melt volume flow rate of the resin composition (MVR) is preferably 2~80cm 3/10 min, more preferably 3~50cm 3/10 min, even more preferably 5 to 20 cm 3/10 min When it shows, favorable surface resistivity can be obtained. The melt volume flow rate of such a resin composition is measured at a cylinder and piston temperature of 300 ° C. and a load of 1.2 kg by a method in accordance with ISO 1133 (JIS K 7210).
本発明の成形品の10kVを印加したときの半減衰時間は10秒以下であり、5秒以下であるものが好ましく、3秒以下がより好ましい。かかる帯電圧半減衰時間が10秒を超えると、帯電した電荷が完全に減衰する前に新たな帯電が発生し、結果としてスパークにいたる電流値が大きくなるため、成形品周辺の精密部品が破壊される可能性が高くなり、好ましくない。なお、成形品の半減衰時間は下記の方法で測定した。すなわち、本発明の導電性樹脂組成物からなる成形品を、スタチックオネストメーター(シシド静電気株式会社製 H−0110)を使用し印加電圧10kVにて測定した。具体的には、成形品から試験片(縦×横×厚み=60mm×50mm×2mm)を3個切削し、温度23℃、湿度50%RHの条件下において前記したスタチックオネストメーターを使用して、試験片面内の中央部の帯電圧半減衰時間を測定し、3個の試験片から得られた値の平均値を試験片の帯電圧半減衰時間とした。 The half decay time of the molded article of the present invention when 10 kV is applied is 10 seconds or less, preferably 5 seconds or less, and more preferably 3 seconds or less. When the half voltage decay time exceeds 10 seconds, a new charge is generated before the charged charge is completely attenuated. As a result, the current value leading to the spark increases, and the precision parts around the molded product are destroyed. The possibility of being increased is not preferable. The half decay time of the molded product was measured by the following method. That is, the molded article made of the conductive resin composition of the present invention was measured at a applied voltage of 10 kV using a static honestometer (H-0110, manufactured by Sisid Electric Co., Ltd.). Specifically, three test pieces (length × width × thickness = 60 mm × 50 mm × 2 mm) were cut from the molded product, and the above-described static one meter was used under the conditions of a temperature of 23 ° C. and a humidity of 50% RH. Then, the half voltage decay time at the center of the test piece surface was measured, and the average value of the values obtained from the three test pieces was taken as the half voltage decay time of the test piece.
以下、実施例により本発明を詳述する。ただし、本発明はこれらに限定されるものではない。 Hereinafter, the present invention will be described in detail by way of examples. However, the present invention is not limited to these.
[実施例1〜10、比較例1〜6]
1.組成物ペレットの製造
下記の方法により、組成物ペレットの製造を行った。
表1に記載の各成分を、表1に示す割合にてドライブレンドした後、径30mmφ、L/D=33.2、混練ゾーン2箇所のスクリューを装備したベント付きニ軸押出機(神戸製鋼所(株)製:KTX30)を用い、シリンダー温度290℃にて溶融混練し、押出し、ストランドカットすることで、各組成物のペレットを得た。
[Examples 1 to 10, Comparative Examples 1 to 6]
1. Production of composition pellets Composition pellets were produced by the following method.
After the components shown in Table 1 were dry blended at the ratios shown in Table 1, a twin screw extruder with a vent (Kobe Steel) equipped with 30 mmφ diameter, L / D = 33.2, and two kneading zone screws. (Commercially available from KTX30) was melt kneaded at a cylinder temperature of 290 ° C., extruded, and strand-cut to obtain pellets of each composition.
2.成形品の作成
かかる樹脂組成物を射出成形により、シリンダー温度290℃、金型温度80℃にて、図1に示す精密部材収納容器を成形し、各種評価に合わせ切削した。
2. Production of Molded Product The resin composition shown in FIG. 1 was molded by injection molding at a cylinder temperature of 290 ° C. and a mold temperature of 80 ° C., and cut according to various evaluations.
3.評価方法
実施例中における各値は下記の方法で求めた。
(1)表面抵抗率
上記の方法で得た成形品をそれぞれの抵抗値に合った抵抗率計を使用して測定した。すなわち、1010Ω/sq以上の場合は、TOA株式会社製 デジタル絶縁計DSM-8103(印加電圧100V、専用プローブ)、107〜1010Ω/sqの場合には、三菱化学株式会社製 ハイレスターUP MCP-HT400(印加電圧100V、UR-SSプローブ(JISK6911準拠))、107Ω/sq以下の場合には、三菱化学株式会社製 ロレスターGP MCP-T600(印加電圧90V、ESPプローブ(JISK7194準拠))を使用した。具体的な測定方法としては、成形品から試験片(縦×横×厚み=90mm×50mm×2mmt)を3個切削し、温度23℃、湿度50%RHの条件下において前記の抵抗率計を使用して試験片面内の中央部の表面抵抗率を測定し3個の試験片から得られた値の平均値を試験片の表面抵抗率とした。
3. Evaluation method Each value in the examples was determined by the following method.
(1) Surface resistivity The molded product obtained by the above method was measured using a resistivity meter suitable for each resistance value. That is, in the case of 10 10 Ω / sq or more, digital insulation meter DSM-8103 (applied voltage 100 V, dedicated probe) manufactured by TOA Co., Ltd., and in the case of 10 7 to 10 10 Ω / sq, manufactured by Mitsubishi Chemical Corporation High Lester UP MCP-HT400 (applied voltage 100V, UR-SS probe (JISK6911 compliant)), 10 7 Ω / sq or less, Lorester GP MCP-T600 (applied voltage 90V, ESP probe (JISK7194) Compliant)). As a specific measurement method, three test pieces (length × width × thickness = 90 mm × 50 mm × 2 mmt) are cut from the molded product, and the above-described resistivity meter is used under the conditions of a temperature of 23 ° C. and a humidity of 50% RH. The surface resistivity of the central part in the test piece surface was measured and the average value of the values obtained from the three test pieces was defined as the surface resistivity of the test piece.
(2)半減衰時間
上記の方法で得た成形品をスタチックオネストメーター(シシド静電気株式会社製 H−0110)を使用し印加電圧10kVにて測定した。具体的には、成形品から試験片(縦×横×厚み=60mm×50mm×2mm)を3個切削し、温度23℃、湿度50%RHの条件下において前記したスタチックオネストメーターを使用して、試験片面内の中央部の帯電圧半減衰時間を測定し、3個の試験片から得られた値の平均値を試験片の帯電圧半減衰時間とした。
(2) Half decay time The molded product obtained by the above method was measured at a applied voltage of 10 kV using a static honestometer (H-0110 manufactured by Sisid Electric Co., Ltd.). Specifically, three test pieces (length × width × thickness = 60 mm × 50 mm × 2 mm) were cut from the molded product, and the above-described static one meter was used under the conditions of a temperature of 23 ° C. and a humidity of 50% RH. Then, the half voltage decay time at the center of the test piece surface was measured, and the average value of the values obtained from the three test pieces was taken as the half voltage decay time of the test piece.
(3)発生ガス量
上記の方法で得た組成物ペレット3gを150℃にて1時間加熱し、ガスクロマトグラム(アジレント社製GC−MS)にて揮発性有機ガス量を測定し、その総量をトルエン換算したものを発生ガス量とした。
(3) Generated gas amount 3 g of the composition pellets obtained by the above method are heated at 150 ° C. for 1 hour, the amount of volatile organic gas is measured with a gas chromatogram (GC-MS manufactured by Agilent), and the total amount is determined. The amount converted to toluene was defined as the amount of generated gas.
(4)スパーク電流
上記の方法で得た成形品を、CDMテスター(阪和電子工業製 HED−C5000)を使用し、JEDEC/JESD22−C101−Cに準拠する方法で、印加電圧2000V/正極1回印加により測定した。具体的には、成形品から試験片(縦×横×厚み=45mm×45mm×2mm)を切削し、温度25℃、湿度50%RHの条件下において前記したCDMテスターを使用して、面内9箇所を5mm間隔でスパーク電流を測定し得られた値の平均値を試験片のスパーク電流とした。このスパーク電流は10A以下であることが必要である。
(4) Spark current Using the CDM tester (HED-C5000, manufactured by Hanwa Denshi Kogyo Co., Ltd.), the molded product obtained by the above method is applied in accordance with JEDEC / JESD22-C101-C. Measured by application. Specifically, a test piece (length × width × thickness = 45 mm × 45 mm × 2 mm) is cut from the molded product, and the above-mentioned CDM tester is used under the conditions of a temperature of 25 ° C. and a humidity of 50% RH. The average value of the values obtained by measuring the spark current at 9 locations at intervals of 5 mm was taken as the spark current of the test piece. This spark current needs to be 10 A or less.
(5)寸法安定性(ヒケ)
上記の方法で得た組成物ペレットを射出成形機(三菱重工業(株)製:80MSP−5)を使用して、シリンダー温度300℃、金型温度80℃にて、測定用の試験片(縦×横×厚み=90mm×50mm×1mmtの成形片)を成形し、ヒケを評価した。ヒケが見られない場合を○、若干のヒケが見られる場合を△、ヒケが見られる場合を×として評価した。
(5) Dimensional stability (sink)
Using the injection molding machine (Mitsubishi Heavy Industries, Ltd. product: 80MSP-5), the composition pellet obtained by said method was measured at the cylinder temperature of 300 degreeC and the mold temperature of 80 degreeC (longitudinal direction). × width × thickness = 90 mm × 50 mm × 1 mmt molded piece), and sink marks were evaluated. The case where no sink marks were observed was evaluated as ◯, the case where some sink marks were observed as Δ, and the case where sink marks were observed as ×.
(6)導電性炭素材料の脱落性
上記の方法で得た組成物ペレットを射出成形機(三菱重工業(株)製:80MSP−5)を使用して、シリンダー温度280℃、金型温度80℃にて、測定用の試験片(直径×高さ=10mm×20mmのピン状成形片)を成形し、往復動摩擦磨耗試験機((株)オリンテック製:AFT−15M)を使用し、23℃、50%RHの条件下において1.5kgの一定荷重の下で台紙の上で往復摩擦させ台紙に付着した導電性炭素材料の脱落跡を評価した。台紙に導電性炭素材料の脱落跡がほとんど見られない場合を○、若干の導電性炭素材料の脱落跡が認められる場合を△、導電性炭素材料の脱落跡がはっきり確認できる場合を×として評価した。
(6) Separability of conductive carbon material Using composition molding pellets obtained by the above method using an injection molding machine (Mitsubishi Heavy Industries, Ltd .: 80MSP-5), cylinder temperature 280 ° C, mold temperature 80 ° C Then, a test specimen for measurement (a pin-shaped molded piece having a diameter × height = 10 mm × 20 mm) was formed, and a reciprocating friction wear tester (manufactured by Olintec Co., Ltd .: AFT-15M) was used at 23 ° C. The trace of the conductive carbon material deposited on the mount by reciprocating friction on the mount under a constant load of 1.5 kg under the condition of 50% RH was evaluated. Evaluated as ◯ when the trace of the conductive carbon material is hardly seen on the mount, △ when the trace of the conductive carbon material is observed as △, and x when the trace of the conductive carbon material can be clearly confirmed did.
(7)流動性
上記の方法で得た組成物ペレットを射出成形機(住友重機械工業(株)製:SG−150U)を使用して、シリンダー温度300℃、金型温度80℃、射出圧力119MPaにて、流路厚1mm、流路幅8mmのアルキメデス型スパイラル長を測定した。上記スパイラル長が10cm以上であるものを○、5〜10であるものを△、5以下であるものを×として評価した。
(7) Fluidity Using the injection molding machine (Sumitomo Heavy Industries, Ltd. product: SG-150U), the cylinder temperature is 300 ° C., the mold temperature is 80 ° C., and the injection pressure is used for the composition pellets obtained by the above method. At 119 MPa, an Archimedean spiral length with a channel thickness of 1 mm and a channel width of 8 mm was measured. The case where the spiral length was 10 cm or more was evaluated as ◯, the case where it was 5-10, and the case where it was 5 or less as x.
(8)外観
上記の方法で得た組成物ペレットを射出成形機(東芝機械(株)製:IS−150EN)を使用して、シリンダー温度280℃、金型温度80℃にて、測定用の試験片(縦×横×厚み=90mm×50mm×2mmtの成形片)を成形し、成形片の表面外観を目視評価した。光沢があり、表面が平滑である場合を◎、表面が平滑である場合を○、若干のざらつきが見られる場合を△、ざらつきが見られる場合を×として評価した。
(8) Appearance Using the injection molding machine (Toshiba Machine Co., Ltd. product: IS-150EN), the composition pellet obtained by the above method was measured at a cylinder temperature of 280 ° C. and a mold temperature of 80 ° C. A test piece (formed piece of length × width × thickness = 90 mm × 50 mm × 2 mmt) was formed, and the surface appearance of the formed piece was visually evaluated. The case where the surface was smooth and the surface was smooth was evaluated as ◎, the case where the surface was smooth was evaluated as ◯, the case where slight roughness was observed, and the case where roughness was observed as ×.
各実施例および比較例の各評価結果を表1〜表2に示した。
なお、実施例及び比較例で使用した原材料は、下記の通りである。
(A成分:芳香族ポリカーボネート)
A−1:芳香族ポリカーボネート(帝人化成株式会社製 L−1225)
(B成分:ポリエチレンテレフタレート)
B−1:ポリエチレンテレフタレート樹脂(帝人株式会社製 TR−4550BH)
(C成分:導電性炭素材料)
C−1:導電性カーボンブラック[ケッチェンブラックEC―600JD(ライオン株式会社製 DBP吸油量495ml/100g、BET比表面積1270m2/g)]
C−2:導電性カーボンブラック[デンカブラック(電気化学工業株式会社製 DBP吸油量191ml/100g、BET比表面積68m2/g)]
C−3:導電性カーボンブラック[MA−600(三菱化学株式会社製 DBP吸油量131ml/100g、BET比表面積140m2/g)]
C−4:カーボンナノチューブ[15重量%カーボンナノチューブマスター MB6015−00(ハイペリオン社製 直径20nm、アスペクト比5以上)]
(D成分:ガラス繊維、ガラスフレーク)
D−1:ガラス繊維[CS 3PE−937(日東紡績株式会社製)]
D−2:ガラスフレーク[REFG−301(日本板硝子株式会社製)]
(E成分:ポリテトラフルオロエチレン粒子)
E−1:ルブロン L−5(ダイキン工業株式会社製)
(F成分:酸化防止剤)
F−1:アデカスタブ PEP−24G(旭電化工業株式会社製)
F−2:TMP(大八化学工業株式会社製)
Tables 1 and 2 show the evaluation results of the examples and comparative examples.
In addition, the raw material used by the Example and the comparative example is as follows.
(Component A: aromatic polycarbonate)
A-1: Aromatic polycarbonate (L-1225 manufactured by Teijin Chemicals Ltd.)
(B component: polyethylene terephthalate)
B-1: Polyethylene terephthalate resin (TR-4550BH manufactured by Teijin Limited)
(C component: conductive carbon material)
C-1: Conductive carbon black [Ketjen Black EC-600JD (manufactured by Lion Corporation, DBP oil absorption 495 ml / 100 g, BET specific surface area 1270 m 2 / g)]
C-2: Conductive carbon black [Denka Black (DBP oil absorption 191 ml / 100 g, BET specific surface area 68 m 2 / g, manufactured by Denki Kagaku Kogyo Co., Ltd.)]
C-3: Conductive carbon black [MA-600 (DBP oil absorption 131 ml / 100 g, BET specific surface area 140 m 2 / g, manufactured by Mitsubishi Chemical Corporation)]
C-4: Carbon nanotube [15 wt% carbon nanotube master MB 6015-00 (Hyperion, diameter 20 nm, aspect ratio 5 or more)]
(D component: glass fiber, glass flake)
D-1: Glass fiber [CS 3PE-937 (manufactured by Nitto Boseki Co., Ltd.)]
D-2: Glass flake [REFG-301 (made by Nippon Sheet Glass Co., Ltd.)]
(E component: polytetrafluoroethylene particles)
E-1: Lubron L-5 (manufactured by Daikin Industries, Ltd.)
(F component: antioxidant)
F-1: ADK STAB PEP-24G (Asahi Denka Kogyo Co., Ltd.)
F-2: TMP (manufactured by Daihachi Chemical Industry Co., Ltd.)
実施例1、実施例2および実施例5に示すように、規定範囲量内のポリエチレンテレフタレートを配合した樹脂組成物からなり、半導電領域である105〜1012Ω/sqの表面抵抗率及び帯電圧半減衰時間を10秒以下に制御した成形品は、成形品表面から発生するスパーク電流を抑制し、成形品の樹脂表面から導電性炭素材料が脱落することを抑制し、更には寸法安定性、流動性、外観にも優れている。なお、実施例1の樹脂組成物におけるメルトボリュームフローレイトは7cm3/10分、実施例2の樹脂組成物は8cm3/10分、実施例5の樹脂組成物は8cm3/10分であり、表面抵抗率を静電領域に制御するために好適な流動性を示す。一方、比較例1の樹脂組成物におけるメルトボリュームフローレイトは1cm3/10分であり、表面抵抗率を静電領域に制御することが困難である。 As shown in Example 1, Example 2 and Example 5, it consists of a resin composition blended with polyethylene terephthalate within a specified range amount, and has a surface resistivity of 10 5 to 10 12 Ω / sq which is a semiconductive region and Molded products with a charged voltage half decay time controlled to 10 seconds or less suppresses spark current generated from the surface of the molded product, prevents the conductive carbon material from falling off from the resin surface of the molded product, and is dimensionally stable. Excellent in properties, fluidity and appearance. Incidentally, melt volume flow rate of the resin composition of Example 1 is 7 cm 3/10 min, the resin composition of Example 2 is 8 cm 3/10 min, the resin composition of Example 5 is 8 cm 3/10 min The fluidity suitable for controlling the surface resistivity in the electrostatic region is exhibited. On the other hand, melt volume flow rate of the resin composition in Comparative Example 1 is 1 cm 3/10 min, it is difficult to control the surface resistivity of the electrostatic area.
比較例1、比較例2、比較例3および比較例4はポリエチレンテレフタレートの配合量が規定範囲外であり、比較例1、比較例2および比較例3のように配合量が少ないと、導電性炭素材料の脱落が十分に抑制できない。一方、比較例4のように配合量が多いと、表面抵抗率が規定範囲内に制御できず、さらに寸法安定性が悪くなり良好な成形品を得ることができない。 In Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4, the blending amount of polyethylene terephthalate is outside the specified range, and if the blending amount is small as in Comparative Example 1, Comparative Example 2 and Comparative Example 3, the conductivity becomes low. The loss of the carbon material cannot be sufficiently suppressed. On the other hand, when the blending amount is large as in Comparative Example 4, the surface resistivity cannot be controlled within the specified range, and the dimensional stability is deteriorated, so that a good molded product cannot be obtained.
比較例5及び比較例6は導電性炭素材料の配合量が規定範囲外であり、比較例5のように配合量が少ないと、半導電領域に表面抵抗率を規定範囲内に制御することが困難であり、スパーク電流も大きい。一方、比較例6のように配合量が多いと、導電性炭素材料の脱落を抑制することができず、流動性も悪い。 In Comparative Example 5 and Comparative Example 6, the compounding amount of the conductive carbon material is outside the specified range. When the compounding amount is small as in Comparative Example 5, the surface resistivity of the semiconductive region can be controlled within the specified range. It is difficult and the spark current is large. On the other hand, when there are many compounding quantities like the comparative example 6, the drop-off | omission of an electroconductive carbon material cannot be suppressed and fluidity | liquidity is also bad.
実施例3、実施例4および実施例6〜10は導電性カーボンブラックの種類を変えた場合、ガラス繊維又はガラスフレークを更に配合した場合、ポリテトラフルオロエチレン粒子を配合した場合、酸化防止剤を配合した場合を示しており、いずれも良好な評価結果を示す。 In Examples 3, 4 and 6 to 10, when the type of conductive carbon black is changed, when glass fiber or glass flake is further blended, when polytetrafluoroethylene particles are blended, an antioxidant is added. The case where it mix | blends is shown and all show a favorable evaluation result.
1:容器本体
2:凹部
1: Container body 2: Recess
Claims (7)
(1) 表面抵抗率が105〜1012Ω/sqである。
(2) 10kVを印加したときの半減衰時間が10秒以下である。 1 to 20 parts by weight of conductive carbon material (C component) with respect to 100 parts by weight of resin component consisting of 55 to 75% by weight (component A) of aromatic polycarbonate resin and 25 to 45% by weight (component B) of polyethylene terephthalate resin A molded product comprising a conductive resin composition contained therein, wherein the molded product satisfies the following (1) and (2), a hard disk related part, an in-process container, an IC chip tray, a wafer transfer container, a glass container, And a molded product comprising a conductive resin composition, wherein the molded product is selected from the group consisting of automotive exterior parts.
(1) The surface resistivity is 10 5 to 10 12 Ω / sq.
(2) The half decay time when 10 kV is applied is 10 seconds or less.
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JP2011016902A (en) * | 2009-07-08 | 2011-01-27 | Teijin Chem Ltd | Molded article comprising conductive resin composition |
JP2017048259A (en) * | 2015-08-31 | 2017-03-09 | 住化スタイロンポリカーボネート株式会社 | Resin-made container member |
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CN104004336B (en) * | 2014-05-05 | 2016-03-30 | 上海锦湖日丽塑料有限公司 | Reduce polycarbonate resin of graphitized carbon black addition and preparation method thereof |
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