JP2017114968A - Polyarylene sulfide resin composition, molded article of the same and method for producing the same - Google Patents
Polyarylene sulfide resin composition, molded article of the same and method for producing the same Download PDFInfo
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- JP2017114968A JP2017114968A JP2015249782A JP2015249782A JP2017114968A JP 2017114968 A JP2017114968 A JP 2017114968A JP 2015249782 A JP2015249782 A JP 2015249782A JP 2015249782 A JP2015249782 A JP 2015249782A JP 2017114968 A JP2017114968 A JP 2017114968A
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- Prior art keywords
- polyarylene sulfide
- sulfide resin
- resin composition
- group
- range
- 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.)
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229920000412 polyarylene Polymers 0.000 title claims abstract description 97
- 239000011342 resin composition Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 89
- 239000011347 resin Substances 0.000 claims abstract description 89
- 239000002608 ionic liquid Substances 0.000 claims abstract description 32
- 239000000155 melt Substances 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 21
- 230000008018 melting Effects 0.000 claims abstract description 21
- 238000000465 moulding Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000004898 kneading Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims description 29
- 125000004432 carbon atom Chemical group C* 0.000 claims description 14
- 239000007822 coupling agent Substances 0.000 claims description 10
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000004183 alkoxy alkyl group Chemical group 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims description 3
- -1 alkali metal salt Chemical class 0.000 description 35
- 238000000034 method Methods 0.000 description 26
- 239000010408 film Substances 0.000 description 25
- 238000012546 transfer Methods 0.000 description 22
- 238000005259 measurement Methods 0.000 description 19
- 239000000047 product Substances 0.000 description 18
- 230000000694 effects Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000006116 polymerization reaction Methods 0.000 description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 9
- 150000001768 cations Chemical class 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 150000001450 anions Chemical class 0.000 description 8
- 239000011231 conductive filler Substances 0.000 description 8
- 239000000835 fiber Substances 0.000 description 8
- 230000001771 impaired effect Effects 0.000 description 8
- 238000001746 injection moulding Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 229910052717 sulfur Inorganic materials 0.000 description 8
- 125000003118 aryl group Chemical group 0.000 description 7
- 239000011541 reaction mixture Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 150000003949 imides Chemical class 0.000 description 6
- 239000012744 reinforcing agent Substances 0.000 description 6
- 125000004434 sulfur atom Chemical group 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 description 5
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 5
- 239000008188 pellet Substances 0.000 description 5
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000004734 Polyphenylene sulfide Substances 0.000 description 4
- 239000007983 Tris buffer Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 125000003710 aryl alkyl group Chemical group 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 238000000748 compression moulding Methods 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 description 4
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 4
- 239000002798 polar solvent Substances 0.000 description 4
- 229920000069 polyphenylene sulfide Polymers 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- IEFUHGXOQSVRDQ-UHFFFAOYSA-N bis(trifluoromethylsulfonyl)azanide;1-methyl-1-propylpiperidin-1-ium Chemical compound CCC[N+]1(C)CCCCC1.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F IEFUHGXOQSVRDQ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 125000005843 halogen group Chemical group 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229920006122 polyamide resin Polymers 0.000 description 3
- 229920005668 polycarbonate resin Polymers 0.000 description 3
- 239000004431 polycarbonate resin Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- HJHUXWBTVVFLQI-UHFFFAOYSA-N tributyl(methyl)azanium Chemical compound CCCC[N+](C)(CCCC)CCCC HJHUXWBTVVFLQI-UHFFFAOYSA-N 0.000 description 3
- 239000004711 α-olefin Substances 0.000 description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 125000003342 alkenyl group Chemical group 0.000 description 2
- 125000000304 alkynyl group Chemical group 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 238000000071 blow moulding Methods 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000007810 chemical reaction solvent Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 125000000753 cycloalkyl group Chemical group 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 150000001991 dicarboxylic acids Chemical class 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 239000002828 fuel tank Substances 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- XTPRURKTXNFVQT-UHFFFAOYSA-N hexyl(trimethyl)azanium Chemical compound CCCCCC[N+](C)(C)C XTPRURKTXNFVQT-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 125000004437 phosphorous atom Chemical group 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000003495 polar organic solvent Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 125000005372 silanol group Chemical group 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- GKNWQHIXXANPTN-UHFFFAOYSA-M 1,1,2,2,2-pentafluoroethanesulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)C(F)(F)F GKNWQHIXXANPTN-UHFFFAOYSA-M 0.000 description 1
- XBWQFDNGNOOMDZ-UHFFFAOYSA-N 1,1,2,2,3,3,3-heptafluoropropane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)F XBWQFDNGNOOMDZ-UHFFFAOYSA-N 0.000 description 1
- KZJUHXVCAHXJLR-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,4-nonafluoro-n-(1,1,2,2,3,3,4,4,4-nonafluorobutylsulfonyl)butane-1-sulfonamide Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F KZJUHXVCAHXJLR-UHFFFAOYSA-N 0.000 description 1
- JGTNAGYHADQMCM-UHFFFAOYSA-M 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F JGTNAGYHADQMCM-UHFFFAOYSA-M 0.000 description 1
- PBMCNXWCDKJXRU-UHFFFAOYSA-N 1-[bis(1,1,2,2,2-pentafluoroethylsulfonyl)methylsulfonyl]-1,1,2,2,2-pentafluoroethane Chemical compound FC(F)(F)C(F)(F)S(=O)(=O)[C-](S(=O)(=O)C(F)(F)C(F)(F)F)S(=O)(=O)C(F)(F)C(F)(F)F PBMCNXWCDKJXRU-UHFFFAOYSA-N 0.000 description 1
- WFKZGXKJFFOGPM-UHFFFAOYSA-N 1-butylthiolan-1-ium Chemical compound CCCC[S+]1CCCC1 WFKZGXKJFFOGPM-UHFFFAOYSA-N 0.000 description 1
- MNHGZSKIAQFMNT-UHFFFAOYSA-N 1-hexylthiolan-1-ium Chemical compound CCCCCC[S+]1CCCC1 MNHGZSKIAQFMNT-UHFFFAOYSA-N 0.000 description 1
- OGLIVJFAKNJZRE-UHFFFAOYSA-N 1-methyl-1-propylpiperidin-1-ium Chemical compound CCC[N+]1(C)CCCCC1 OGLIVJFAKNJZRE-UHFFFAOYSA-N 0.000 description 1
- VIAXSPFGGOUOOQ-UHFFFAOYSA-N 1-pentylthiolan-1-ium Chemical compound CCCCC[S+]1CCCC1 VIAXSPFGGOUOOQ-UHFFFAOYSA-N 0.000 description 1
- ITFNVRYJMKTWPL-UHFFFAOYSA-N 1-propylthiolan-1-ium Chemical compound CCC[S+]1CCCC1 ITFNVRYJMKTWPL-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- IMSODMZESSGVBE-UHFFFAOYSA-N 2-Oxazoline Chemical compound C1CN=CO1 IMSODMZESSGVBE-UHFFFAOYSA-N 0.000 description 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- ZWRMFEQRSUWLKC-UHFFFAOYSA-N 2-hydroxyethyl(tripropyl)azanium Chemical compound CCC[N+](CCC)(CCC)CCO ZWRMFEQRSUWLKC-UHFFFAOYSA-N 0.000 description 1
- DVSPHWCZXKPJEQ-UHFFFAOYSA-N 2-methoxyethyl(trimethyl)azanium Chemical compound COCC[N+](C)(C)C DVSPHWCZXKPJEQ-UHFFFAOYSA-N 0.000 description 1
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 description 1
- NNTRMVRTACZZIO-UHFFFAOYSA-N 3-isocyanatopropyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)CCCN=C=O NNTRMVRTACZZIO-UHFFFAOYSA-N 0.000 description 1
- VZXOZSQDJJNBRC-UHFFFAOYSA-N 4-chlorobenzenethiol Chemical compound SC1=CC=C(Cl)C=C1 VZXOZSQDJJNBRC-UHFFFAOYSA-N 0.000 description 1
- NWORVTSPNLVHSH-UHFFFAOYSA-N 4-ethyl-4-methylmorpholin-4-ium Chemical compound CC[N+]1(C)CCOCC1 NWORVTSPNLVHSH-UHFFFAOYSA-N 0.000 description 1
- OSSMYOQKNHMTIP-UHFFFAOYSA-N 5-[dimethoxy(methyl)silyl]pentane-1,3-diamine Chemical compound CO[Si](C)(OC)CCC(N)CCN OSSMYOQKNHMTIP-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- 235000010893 Bischofia javanica Nutrition 0.000 description 1
- 240000005220 Bischofia javanica Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004739 DIC.PPS Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 description 1
- 239000004420 Iupilon Substances 0.000 description 1
- 239000004997 Liquid crystal elastomers (LCEs) Substances 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- GSBKRFGXEJLVMI-UHFFFAOYSA-N Nervonyl carnitine Chemical compound CCC[N+](C)(C)C GSBKRFGXEJLVMI-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NQRYJNQNLNOLGT-UHFFFAOYSA-O Piperidinium(1+) Chemical compound C1CC[NH2+]CC1 NQRYJNQNLNOLGT-UHFFFAOYSA-O 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 1
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- UCVGPWMKVFBRMN-UHFFFAOYSA-N tributyl(2-hydroxyethyl)azanium Chemical compound CCCC[N+](CCO)(CCCC)CCCC UCVGPWMKVFBRMN-UHFFFAOYSA-N 0.000 description 1
- WODRZXVHZAQLGS-UHFFFAOYSA-N tributyl(hydroxymethyl)azanium Chemical compound CCCC[N+](CO)(CCCC)CCCC WODRZXVHZAQLGS-UHFFFAOYSA-N 0.000 description 1
- DDBUVUBWJVIGFH-UHFFFAOYSA-N trichloro(3-isocyanatopropyl)silane Chemical compound Cl[Si](Cl)(Cl)CCCN=C=O DDBUVUBWJVIGFH-UHFFFAOYSA-N 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
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- GZBUMTPCIKCWFW-UHFFFAOYSA-N triethylcholine Chemical compound CC[N+](CC)(CC)CCO GZBUMTPCIKCWFW-UHFFFAOYSA-N 0.000 description 1
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- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 description 1
- FFZLLDUIDGLEQA-UHFFFAOYSA-N trimethyl(pent-2-enoyl)azanium Chemical compound C(C)C=CC(=O)[N+](C)(C)C FFZLLDUIDGLEQA-UHFFFAOYSA-N 0.000 description 1
- OZHHAAKCLPQJDD-UHFFFAOYSA-N tris(2-methoxyethyl)-methylazanium Chemical compound COCC[N+](C)(CCOC)CCOC OZHHAAKCLPQJDD-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 239000000326 ultraviolet stabilizing agent Substances 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- 150000007934 α,β-unsaturated carboxylic acids Chemical class 0.000 description 1
Abstract
Description
本発明はポリアリーレンスルフィド樹脂組成物、前記樹脂を成形してなる成形品、および前記樹脂の製造方法に関するものである。 The present invention relates to a polyarylene sulfide resin composition, a molded product obtained by molding the resin, and a method for producing the resin.
ポリフェニレンスルフィド樹脂（以下、「ＰＰＳ樹脂」と略すことがある）に代表されるポリアリーレンスルフィド樹脂（以下、「ＰＡＳ樹脂」と略すことがある）は、優れた耐熱性、難燃性、剛性、耐薬品性、電気絶縁性など、エンジニアリングプラスチックとして好適な性質を有しており、射出成形用を中心として各種電気・電子部品、機械部品および自動車部品などに使用されている。 A polyarylene sulfide resin (hereinafter sometimes abbreviated as “PAS resin”) represented by a polyphenylene sulfide resin (hereinafter sometimes abbreviated as “PPS resin”) has excellent heat resistance, flame retardancy, rigidity, It has suitable properties as an engineering plastic such as chemical resistance and electrical insulation, and is used for various electrical / electronic parts, mechanical parts, automobile parts, etc. mainly for injection molding.
各種樹脂と導電性フィラーの混練物である導電コンパウンドは、静電破壊の防止や、静電吸着による埃の付着を防止することを目的として半導体や精密部品の搬送容器、導電性を活かしたプリンター、複写機用の印刷ロールなどに用いられ、また静電気による引火防止を目的とした燃料タンクやチューブ、導電糸を用いた静電対策用衣料に用いられている。 Conductive compound, which is a kneaded mixture of various resins and conductive fillers, is a transport container for semiconductors and precision parts, and a printer that takes advantage of electrical conductivity to prevent electrostatic breakdown and dust adhesion due to electrostatic adsorption. It is used for printing rolls for copying machines, etc., and for antistatic clothing using fuel tanks, tubes, and conductive yarns for the purpose of preventing ignition by static electricity.
これら導電コンパウンドに用いる導電性フィラーとしてはカーボンブラック（以下、ＣＢと略すことがある）が汎用の原料であるが、ＣＢ単独で充分な導電性を得ようとすると配合量が増加し、ＣＢが樹脂組成物中に均一に分散しない傾向となる。その結果、凝集などが生じた場合には所望の導電性が得られないばかりでなく、表面外観の悪化などが起こることになる。このため、ＣＢの混練時に添加するＣＢの選定、混練方法、混練条件、添加剤など様々な条件、方法が検討されている。 As a conductive filler used in these conductive compounds, carbon black (hereinafter sometimes abbreviated as CB) is a general-purpose raw material. However, if CB alone is used to obtain sufficient conductivity, the blending amount increases, and CB is reduced. It tends to not be uniformly dispersed in the resin composition. As a result, when aggregation or the like occurs, not only the desired conductivity cannot be obtained, but also the surface appearance is deteriorated. For this reason, various conditions and methods, such as selection of CB to be added at the time of CB kneading, kneading method, kneading conditions, and additives, have been studied.
また、ポリアリーレンスルフィド樹脂に対するＣＢの分散性が優れているとは言えず、押出し成形時にＣＢの分散状態が変化し、導電性が不均一となる問題も抱えていた。このように導電性が不均一である場合に、転写ベルトなどに用いると、印刷時に文字の中抜けやトナーの飛び散りが発生するという課題が存在した。このように半導体領域においてＣＢを用いてポリアリーレンスルフィド樹脂に均一かつ十分な導電性を付与することは困難であった。 Moreover, it cannot be said that the dispersibility of CB with respect to the polyarylene sulfide resin is excellent, and the dispersion state of CB is changed at the time of extrusion molding, and there is a problem that the conductivity becomes non-uniform. Thus, when the conductivity is non-uniform, when used for a transfer belt or the like, there is a problem in that characters are lost during printing or toner is scattered. Thus, it has been difficult to impart uniform and sufficient conductivity to the polyarylene sulfide resin using CB in the semiconductor region.
そこで、ポリアリーレンスルフィド樹脂にポリアミド樹脂を配合することで、樹脂の靱性を高めつつ、かつ樹脂組成物中のカーボンの分散状態を均一にして、比較的均一な導電性が付与された電子写真用転写ベルトが得られることが報告されている（特許文献１、２参照）。しかしながら、ポリアミド樹脂による導電性材料の分散性能は十分なものとは言えず、その結果、成形品の表面方向の導電性（表面抵抗率）や厚み方向の導電性（体積抵抗率）にばらつきが生じていた。 Therefore, by blending a polyamide resin with a polyarylene sulfide resin, the toughness of the resin is increased, and the dispersion state of carbon in the resin composition is made uniform to provide relatively uniform conductivity. It has been reported that a transfer belt can be obtained (see Patent Documents 1 and 2). However, it cannot be said that the dispersion performance of the conductive material by the polyamide resin is sufficient, and as a result, there are variations in the surface direction conductivity (surface resistivity) and the thickness direction conductivity (volume resistivity) of the molded product. It was happening.
従って本発明が解決しようとする課題は、表面及び厚み方向における導電性のばらつきが抑制され、均一かつ十分な導電性が付与されたポリアリーレンスルフィド樹脂組成物、該樹脂組成物を成形した成形品、及びポリアリーレンスルフィド樹脂組成物の製造方法を提供することを課題とする。 Therefore, the problem to be solved by the present invention is that a polyarylene sulfide resin composition in which variation in conductivity in the surface and thickness direction is suppressed and uniform and sufficient conductivity is imparted, and a molded article obtained by molding the resin composition And a method for producing a polyarylene sulfide resin composition.
本発明者等は、上記の課題を解決するため鋭意研究を重ねた結果、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂にイオン液体を添加して用いることで、均一かつ十分な導電性が付与されたポリアリーレンスルフィド樹脂組成物が得られることを見出し、上記課題を解決するに至った。 As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that an ionic liquid is added to a polyarylene sulfide resin having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s]. It has been found that a polyarylene sulfide resin composition having uniform and sufficient conductivity can be obtained by adding and using the above, and has solved the above problems.
すなわち、本発明は、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）と、イオン液体（Ｂ）を必須成分として配合してなることを特徴とするポリアリーレンスルフィド樹脂組成物に関する。 That is, the present invention comprises blending polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. of 5 to 1000 [Pa · s] and an ionic liquid (B) as essential components. The present invention relates to a polyarylene sulfide resin composition.
さらに本発明は、前記ポリアリーレンスルフィド樹脂組成物を成形してなることを特徴とする成形品に関する。 Furthermore, the present invention relates to a molded product obtained by molding the polyarylene sulfide resin composition.
さらに本発明は、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）と、イオン液体（Ｂ）を必須成分として、ポリアリーレンスルフィド樹脂（Ａ）の融点以上で溶融混練することを特徴とするポリアリーレンスルフィド樹脂組成物の製造方法に関する。 Furthermore, the present invention provides a polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s] and an ionic liquid (B) as essential components. It is related with the manufacturing method of the polyarylene sulfide resin composition characterized by melt-kneading above melting | fusing point of resin (A).
本発明によれば、表面及び厚み方向における導電性のばらつきが抑制され、均一かつ十分な導電性が付与されたポリアリーレンスルフィド樹脂、該樹脂組成物を成形した成形品、及びポリアリーレンスルフィド樹脂組成物の製造方法を提供することができる。 According to the present invention, polyarylene sulfide resin in which variation in conductivity in the surface and thickness direction is suppressed and uniform and sufficient conductivity is imparted, a molded product obtained by molding the resin composition, and polyarylene sulfide resin composition A method for manufacturing a product can be provided.
本発明のポリアリーレンスルフィド樹脂組成物は、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）と、イオン液体（Ｂ）を必須成分として配合してなることを特徴とする。 The polyarylene sulfide resin composition of the present invention requires a polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s] and an ionic liquid (B). It is characterized by being blended as a component.
＜３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）＞
本発明のポリアリーレンスルフィド樹脂組成物は、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）を必須成分として配合してなる。
本発明に使用する前記ポリアリーレンスルフィド樹脂は、芳香族環と硫黄原子とが結合した構造を繰り返し単位とする樹脂構造を有するものであり、具体的には、下記式（１）
<Polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s]>
The polyarylene sulfide resin composition of the present invention comprises a polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s] as an essential component.
The polyarylene sulfide resin used in the present invention has a resin structure having a repeating unit of a structure in which an aromatic ring and a sulfur atom are bonded. Specifically, the polyarylene sulfide resin has the following formula (1):
ここで、前記式（１）で表される構造部位は、特に該式中のＲ１及びＲ２は、前記ポリアリーレンスルフィド樹脂の機械的強度の点から水素原子であることが好ましく、その場合、下記式（２）で表されるパラ位で結合するものが好ましいものとして挙げられる。 Here, in the structural site represented by the formula (1), R 1 and R 2 in the formula are preferably hydrogen atoms from the viewpoint of the mechanical strength of the polyarylene sulfide resin. A compound bonded at the para position represented by the following formula (2) is preferable.
また、前記ポリアリーレンスルフィド樹脂は、前記式（１）で表される構造部位のみならず、下記の構造式（３）〜（６） Further, the polyarylene sulfide resin is not only the structural portion represented by the formula (1), but also the following structural formulas (3) to (6).
また、前記ポリアリーレンスルフィド樹脂は、その分子構造中に、下記式（７） The polyarylene sulfide resin has the following formula (7) in its molecular structure.
また、ポリアリーレンスルフィド樹脂の物性は、本発明の効果を損ねない限り特に限定されないが、以下の通りである。 The physical properties of the polyarylene sulfide resin are not particularly limited as long as the effects of the present invention are not impaired, but are as follows.
（溶融粘度）
本発明に用いるポリアリーレンスルフィド樹脂は、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であり、このうち１０〜５００〔Ｐａ・ｓ〕の範囲が好ましく、更に１５〜３５０〔Ｐａ・ｓ〕の範囲がより好ましい、特に本発明の樹脂組成物をフィルム又はシートに成形する場合には１００〜３５０〔Ｐａ・ｓ〕の範囲が最も好ましい。ただし、３００℃で測定した溶融粘度（Ｖ６）とは、高化式フローテスター（島津製作所製「ＣＦＴ−５００Ｄ」）を用いて、温度３００℃、荷重１．９６ＭＰａ、オリフィス長／オリフィス径の比が１０／１であるオリフィス（長さ１０．０±０．００５ｍｍ、穴径１．０±０．０１ｍｍの標準付属オリフィス（ダイ））を使用して６分間保持した後に測定した溶融粘度を表す。
(Melt viscosity)
The polyarylene sulfide resin used in the present invention has a melt viscosity (V6) measured at 300 ° C. of 5 to 1000 [Pa · s], preferably 10 to 500 [Pa · s]. The range of 15 to 350 [Pa · s] is more preferable, and the range of 100 to 350 [Pa · s] is most preferable particularly when the resin composition of the present invention is formed into a film or sheet. However, the melt viscosity (V6) measured at 300 ° C. is a ratio of 300 ° C., load 1.96 MPa, orifice length / orifice diameter using a Koka flow tester (“CFT-500D” manufactured by Shimadzu Corporation). Represents melt viscosity measured after holding for 6 minutes using an orifice with a length of 10 ± 1 (standard attached orifice (die) with a length of 10.0 ± 0.005 mm and a hole diameter of 1.0 ± 0.01 mm) .
（非ニュートン指数）
本発明に用いる前記ポリアリーレンスルフィド樹脂の非ニュートン指数は、０．９０〜２．００の範囲であることが好ましい。リニア型ポリアリーレンスルフィド樹脂を用いる場合には、非ニュートン指数が０．９０〜１．５０の範囲であることが好ましく、さらに０．９５〜１．２０の範囲であることがより好ましい。このようなポリアリーレンスルフィド樹脂は機械的物性、流動性、耐磨耗性に優れる。ただし、非ニュートン指数（Ｎ値）は、キャピログラフを用いて３００℃、オリフィス長（Ｌ）とオリフィス径（Ｄ）の比、Ｌ／Ｄ＝４０の条件下で、剪断速度及び剪断応力を測定し、下記式を用いて算出した値である。
(Non-Newtonian index)
The non-Newtonian index of the polyarylene sulfide resin used in the present invention is preferably in the range of 0.90 to 2.00. When the linear polyarylene sulfide resin is used, the non-Newton index is preferably in the range of 0.90 to 1.50, and more preferably in the range of 0.95 to 1.20. Such a polyarylene sulfide resin is excellent in mechanical properties, fluidity, and abrasion resistance. However, the non-Newtonian index (N value) is measured by measuring the shear rate and shear stress using a capillograph at 300 ° C, the ratio of the orifice length (L) to the orifice diameter (D), and L / D = 40. These are values calculated using the following formula.
（製造方法）
前記ポリアリーレンスルフィド樹脂（Ａ）の製造方法としては、特に限定されないが、例えば１）硫黄と炭酸ソーダの存在下でジハロゲノ芳香族化合物を、必要ならばポリハロゲノ芳香族化合物ないしその他の共重合成分を加えて、重合させる方法、２）極性溶媒中でスルフィド化剤等の存在下にジハロゲノ芳香族化合物を、必要ならばポリハロゲノ芳香族化合物ないしその他の共重合成分を加えて、重合させる方法、３）ｐ−クロルチオフェノールを、必要ならばその他の共重合成分を加えて、自己縮合させる方法、等が挙げられる。これらの方法のなかでも、２）の方法が汎用的であり好ましい。反応の際に、重合度を調節するためにカルボン酸やスルホン酸のアルカリ金属塩を添加したり、水酸化アルカリを添加しても良い。上記２）方法のなかでも、加熱した有機極性溶媒とジハロゲノ芳香族化合物とを含む混合物に含水スルフィド化剤を水が反応混合物から除去され得る速度で導入し、有機極性溶媒中でジハロゲノ芳香族化合物とスルフィド化剤とを、必要に応じてポリハロゲノ芳香族化合物と加え、反応させること、及び反応系内の水分量を該有機極性溶媒１モルに対して０．０２〜０．５モルの範囲にコントロールすることによりポリアリーレンスルフィド樹脂を製造する方法（特開平０７−２２８６９９号公報参照。）や、固形のアルカリ金属硫化物及び非プロトン性極性有機溶媒の存在下でジハロゲノ芳香族化合物と必要ならばポリハロゲノ芳香族化合物ないしその他の共重合成分を加え、アルカリ金属水硫化物及び有機酸アルカリ金属塩を、硫黄源１モルに対して０．０１〜０．９モルの有機酸アルカリ金属塩および反応系内の水分量を非プロトン性極性有機溶媒１モルに対して０．０２モル以下の範囲にコントロールしながら反応させる方法（ＷＯ２０１０／０５８７１３号パンフレット参照。）で得られるものが特に好ましい。ジハロゲノ芳香族化合物の具体的な例としては、ｐ−ジハロベンゼン、ｍ−ジハロベンゼン、ｏ−ジハロベンゼン、２，５−ジハロトルエン、１，４−ジハロナフタレン、１−メトキシ−２，５−ジハロベンゼン、４，４’−ジハロビフェニル、３，５−ジハロ安息香酸、２，４−ジハロ安息香酸、２，５−ジハロニトロベンゼン、２，４−ジハロニトロベンゼン、２，４−ジハロアニソール、ｐ，ｐ’−ジハロジフェニルエーテル、４，４’−ジハロベンゾフェノン、４，４’−ジハロジフェニルスルホン、４，４’−ジハロジフェニルスルホキシド、４，４’−ジハロジフェニルスルフィド、及び、上記各化合物の芳香環に炭素原子数１〜１８のアルキル基を有する化合物が挙げられ、ポリハロゲノ芳香族化合物としては１，２，３−トリハロベンゼン、１，２，４−トリハロベンゼン、１，３，５−トリハロベンゼン、１，２，３，５−テトラハロベンゼン、１，２，４，５−テトラハロベンゼン、１，４，６−トリハロナフタレンなどが挙げられる。また、上記各化合物中に含まれるハロゲン原子は、塩素原子、臭素原子であることが望ましい。
(Production method)
The method for producing the polyarylene sulfide resin (A) is not particularly limited. For example, 1) dihalogenoaromatic compound in the presence of sulfur and sodium carbonate, and if necessary polyhalogenoaromatic compound or other copolymerization component. In addition, a polymerization method, 2) a dihalogenoaromatic compound in a polar solvent in the presence of a sulfidizing agent, and a polyhalogenoaromatic compound or other copolymerization component, if necessary, and polymerization, 3) Examples of the method include self-condensation of p-chlorothiophenol by adding another copolymer component if necessary. Among these methods, the method 2) is versatile and preferable. During the reaction, or by adding an alkali metal salt of a carboxylic acid or sulfonic acid to adjust the degree of polymerization, it may be added alkali hydroxide. Among the above methods 2), a hydrous sulfiding agent is introduced into a mixture containing a heated organic polar solvent and a dihalogenoaromatic compound at a rate at which water can be removed from the reaction mixture, and the dihalogenoaromatic compound in the organic polar solvent. And a sulfidizing agent, if necessary, with a polyhalogenoaromatic compound and reacting, and the amount of water in the reaction system is in the range of 0.02 to 0.5 mol with respect to 1 mol of the organic polar solvent. If necessary, a method for producing a polyarylene sulfide resin by controlling (see JP 07-228699 A), a dihalogenoaromatic compound in the presence of a solid alkali metal sulfide and an aprotic polar organic solvent, if necessary Polyhalogenoaromatic compound or other copolymerization component is added, and alkali metal hydrosulfide and organic acid alkali metal salt are added to sulfur source 1 The organic acid alkali metal salt in an amount of 0.01 to 0.9 mol and the amount of water in the reaction system are controlled in a range of 0.02 mol or less with respect to 1 mol of the aprotic polar organic solvent. Those obtained by the method (see pamphlet of WO2010 / 058713) are particularly preferred. Specific examples of the dihalogenoaromatic compound include p-dihalobenzene, m-dihalobenzene, o-dihalobenzene, 2,5-dihalotoluene, 1,4-dihalonaphthalene, 1-methoxy-2,5-dihalobenzene, 4, 4'-dihalobiphenyl, 3,5-dihalobenzoic acid, 2,4-dihalobenzoic acid, 2,5-dihalonitrobenzene, 2,4-dihalonitrobenzene, 2,4-dihaloanisole, p, p '-Dihalodiphenyl ether, 4,4'-dihalobenzophenone, 4,4'-dihalodiphenyl sulfone, 4,4'-dihalodiphenyl sulfoxide, 4,4'-dihalodiphenyl sulfide, and each of the above compounds include compounds having an aromatic ring in the alkyl group having 1 to 18 carbon atoms. Examples of the Poriharogeno aromatics 1,2,3 Toriharobe Zen, 1,2,4-trihalobenzene, 1,3,5-trihalobenzene, 1,2,3,5-tetrahalobenzene, 1,2,4,5-tetrahalobenzene, 1,4,6- And trihalonaphthalene. Moreover, it is desirable that the halogen atom contained in each compound is a chlorine atom or a bromine atom.
重合工程により得られたポリアリーレンスルフィド樹脂を含む反応混合物の後処理方法としては、特に制限されるものではないが、例えば、（１）重合反応終了後、先ず反応混合物をそのまま、あるいは酸または塩基を加えた後、減圧下または常圧下で溶媒を留去し、次いで溶媒留去後の固形物を水、反応溶媒（又は低分子ポリマーに対して同等の溶解度を有する有機溶媒）、アセトン、メチルエチルケトン、アルコール類などの溶媒で１回または２回以上洗浄し、更に中和、水洗、濾過および乾燥する方法、或いは、（２）重合反応終了後、反応混合物に水、アセトン、メチルエチルケトン、アルコール類、エーテル類、ハロゲン化炭化水素、芳香族炭化水素、脂肪族炭化水素などの溶媒（使用した重合溶媒に可溶であり、かつ少なくともポリアリーレンスルフィドに対しては貧溶媒である溶媒）を沈降剤として添加して、ポリアリーレンスルフィドや無機塩等の固体状生成物を沈降させ、これらを濾別、洗浄、乾燥する方法、或いは、（３）重合反応終了後、反応混合物に反応溶媒（又は低分子ポリマーに対して同等の溶解度を有する有機溶媒）を加えて撹拌した後、濾過して低分子量重合体を除いた後、水、アセトン、メチルエチルケトン、アルコール類などの溶媒で１回または２回以上洗浄し、その後中和、水洗、濾過および乾燥をする方法、（４）重合反応終了後、反応混合物に水を加えて水洗浄、濾過、必要に応じて水洗浄の時に酸を加えて酸処理し、乾燥をする方法、（５）重合反応終了後、反応混合物を濾過し、必要に応じ、反応溶媒で１回または２回以上洗浄し、更に水洗浄、濾過および乾燥する方法、等が挙げられる。 The post-treatment method of the reaction mixture containing the polyarylene sulfide resin obtained by the polymerization step is not particularly limited. For example, (1) after the completion of the polymerization reaction, the reaction mixture is left as it is, or an acid or a base is used. After adding the solvent, the solvent is distilled off under reduced pressure or normal pressure, and then the solid after the solvent is distilled off is water, a reaction solvent (or an organic solvent having an equivalent solubility in a low molecular weight polymer), acetone, methyl ethyl ketone. , A method of washing once or twice with a solvent such as alcohols, and further neutralizing, washing with water, filtering and drying, or (2) after completion of the polymerization reaction, water, acetone, methyl ethyl ketone, alcohols, Solvents such as ethers, halogenated hydrocarbons, aromatic hydrocarbons, aliphatic hydrocarbons (soluble in the polymerization solvent used, and at least A solvent which is a poor solvent for the arylene sulfide) is added as a precipitating agent to precipitate solid products such as polyarylene sulfide and inorganic salts, and these are filtered, washed and dried, or (3) After the completion of the polymerization reaction, the reaction mixture (or an organic solvent having an equivalent solubility with respect to the low molecular polymer) is added to the reaction mixture and stirred, and then filtered to remove the low molecular weight polymer. A method of washing once or twice with a solvent such as acetone, methyl ethyl ketone, alcohol, etc., followed by neutralization, washing with water, filtration and drying. (4) After completion of the polymerization reaction, water is added to the reaction mixture to wash with water. Filtration, if necessary, acid treatment at the time of washing with water, acid treatment and drying, (5) after completion of the polymerization reaction, the reaction mixture is filtered, and if necessary, once or twice or more with a reaction solvent Wash Further washing with water, a method of filtering and drying, and the like.
尚、上記（１）〜（５）に例示したような後処理方法において、ポリアリーレンスルフィド樹脂の乾燥は真空中で行なってもよいし、空気中あるいは窒素のような不活性ガス雰囲気中で行なってもよい。 In the post-treatment methods exemplified in the above (1) to (5), the polyarylene sulfide resin may be dried in a vacuum or in an inert gas atmosphere such as air or nitrogen. May be.
＜イオン液体（Ｂ）＞
本発明のポリアリーレンスルフィド樹脂組成物は、イオン液体（Ｂ）を必須成分として配合してなる。
本発明に用いるイオン液体は、カチオン（陽イオン）とアニオン（陰イオン）とから構成され、一般に融点が約１００℃以下、すなわち約１００℃以下で液体である物質を指す。また、融点が室温以下の場合でも溶融状態である化合物が存在することから常温溶融塩または室温溶融塩と呼ばれる場合もある。イオン液体のカチオンおよび／またはアニオンは立体的に比較的嵩高く、通常これらの一方および／または両方は有機イオンである。イオン液体は、公知の方法、例えばアニオン交換法、酸エステル法、中和法などの方法により合成することができる。
<Ionic liquid (B)>
The polyarylene sulfide resin composition of the present invention is formed by blending the ionic liquid (B) as an essential component.
The ionic liquid used in the present invention refers to a substance composed of a cation (cation) and an anion (anion) and generally having a melting point of about 100 ° C. or lower, that is, about 100 ° C. or lower. Further, even when the melting point is not higher than room temperature, a compound that is in a molten state exists, so it may be called a room temperature molten salt or a room temperature molten salt. The cations and / or anions of the ionic liquid are sterically relatively bulky and usually one and / or both of these are organic ions. The ionic liquid can be synthesized by a known method such as an anion exchange method, an acid ester method, or a neutralization method.
イオン液体に含まれるカチオンとしては、アンモニウムイオン、ホスホニウムイオン、スルホニウムイオンなどを用いてよい。アンモニウムイオンとしては、アルキルアンモニウム、イミダゾリウム、ピリジニウム、ピロリジニウム、ピロリニウム、ピラジニウム、ピリミジニウム、トリアゾニウム、トリアジニウム、キノリニウム、イソキノリニウム、インドリニウム、キノキサリニウム、ピペリジニウム、オキサゾリニウム、チアゾリニウム、モルホリニウム、ピペラジニウム、およびそれらの組み合わせからなる群から選択されるアンモニウムイオンが挙げられる。ホスホニウムイオンとしては、テトラアルキルホスホニウム、アリールホスホニウム、アルキルアリールホスホニウムおよびそれらの組み合わせからなる群から選択されるホスホニウムイオンなどが挙げられる。スルホニウムイオンとしては、アルキルスルホニウム、アリールスルホニウム、チオフェニウム、テトラヒドロチオフェニウムおよびそれらの組み合わせからなる群から選択されるスルホニウムイオンなどが挙げられる。 As the cation contained in the ionic liquid, ammonium ion, phosphonium ion, sulfonium ion, or the like may be used. Ammonium ions include alkylammonium, imidazolium, pyridinium, pyrrolidinium, pyrrolium, pyrazinium, pyrimidinium, triazonium, triazinium, quinolinium, isoquinolinium, indolinium, quinoxalinium, piperidinium, oxazolinium, thiazolinium, morpholinium, piperazinium, and combinations thereof Examples include ammonium ions selected from the group. Examples of phosphonium ions include phosphonium ions selected from the group consisting of tetraalkylphosphonium, arylphosphonium, alkylarylphosphonium, and combinations thereof. Examples of the sulfonium ion include a sulfonium ion selected from the group consisting of alkylsulfonium, arylsulfonium, thiophenium, tetrahydrothiophenium, and combinations thereof.
上記カチオンにおいて窒素原子、リン原子または硫黄原子に直接結合するアルキル基は、直鎖、分岐または環式の、炭素原子数１〜２０、１〜１２または１〜８のアルキル基とすることができる。窒素原子、リン原子または硫黄原子に直接結合するアリール基は、単環式または縮合環式の、炭素原子数５〜２０のアリール基とすることができる。これらのカチオンを構成する構造中の任意の部位が、アルキル基、アルケニル基、アルキニル基、シクロアルキル基、アリール基、アラルキル基、アリールアルキル基、アルコキシ基、アリールオキシ基、水酸基、カルボニル基、カルボキシル基、エステル基、アシル基、アミノ基、アミド基、イミノ基、イミド基、ニトロ基、ニトリル基、スルフィド基、スルホキシド基、スルホン基、ハロゲン原子などでさらに置換されていてもよく、カチオンを構成する構造の主鎖または環に酸素原子、窒素原子、硫黄原子、ケイ素原子などのヘテロ原子が含まれてもよい。本発明のイオン液体のカチオン部としてはアンモニウムイオンが好ましい。 The alkyl group directly bonded to the nitrogen atom, phosphorus atom or sulfur atom in the cation can be a linear, branched or cyclic alkyl group having 1 to 20, 1 to 12 or 1 to 8 carbon atoms. . The aryl group directly bonded to the nitrogen atom, phosphorus atom or sulfur atom can be a monocyclic or condensed cyclic aryl group having 5 to 20 carbon atoms. Arbitrary sites in the structure constituting these cations are alkyl groups, alkenyl groups, alkynyl groups, cycloalkyl groups, aryl groups, aralkyl groups, arylalkyl groups, alkoxy groups, aryloxy groups, hydroxyl groups, carbonyl groups, carboxyls. Group, ester group, acyl group, amino group, amide group, imino group, imide group, nitro group, nitrile group, sulfide group, sulfoxide group, sulfone group, halogen atom, etc. The main chain or ring of the structure may contain a hetero atom such as an oxygen atom, a nitrogen atom, a sulfur atom, or a silicon atom. As a cation part of the ionic liquid of the present invention, an ammonium ion is preferable.
カチオンの具体例としては、Ｎ−メチル−Ｎ，Ｎ，Ｎ−トリブチルアンモニウム、Ｎ−エチル−Ｎ’−メチルイミダゾリウム、Ｎ−メチル−Ｎ−プロピルピペリジニウム、Ｎ，Ｎ，Ｎ−トリメチル−Ｎ−プロピルアンモニウム、Ｎ−メチル−Ｎ，Ｎ，Ｎ−トリプロピルアンモニウム、Ｎ，Ｎ，Ｎ−トリメチル−Ｎ−ブチルアンモニウム、Ｎ，Ｎ，Ｎ−トリメチル−Ｎ−メトキシエチルアンモニウム、Ｎ−メチル−Ｎ，Ｎ，Ｎ−トリス（メトキシエチル）アンモニウム、Ｎ，Ｎ−ジメチル−Ｎ−ブチル−Ｎ−メトキシエチルアンモニウム、Ｎ，Ｎ−ジメチル−Ｎ，Ｎ−ジブチルアンモニウム、Ｎ−メチル−Ｎ，Ｎ−ジブチル−Ｎ−メトキシエチルアンモニウム、Ｎ，Ｎ，Ｎ−トリメチル−Ｎ−ヘキシルアンモニウム、Ｎ，Ｎ−ジエチル−Ｎ−メチル−Ｎ−（２−メトキシエチル）アンモニウム、１−プロピル−テトラヒドロチオフェニウム、１−ブチル−テトラヒドロチオフェニウム、１−ペンチル−テトラヒドロチオフェニウム、１−ヘキシル−テトラヒドロチオフェニウム、グリシジルトリメチルアンモニウム、Ｎ−エチルアクリロイル−Ｎ，Ｎ，Ｎ−トリメチルアンモニウム、Ｎ−エチル−Ｎ−メチルモルホリニウム、Ｎ，Ｎ，Ｎ−トリオクチルアンモニウム、Ｎ−メチル−Ｎ，Ｎ，Ｎ−トリオクチルアンモニウム、Ｎ−ヒドロキシメチル−Ｎ，Ｎ，Ｎ−トリメチルアンモニウム、Ｎ−ヒドロキシメチル−Ｎ，Ｎ，Ｎ−トリエチルアンモニウム、Ｎ−ヒドロキシメチル−Ｎ，Ｎ，Ｎ−トリブチルアンモニウム、Ｎ−ヒドロキシメチル−Ｎ，Ｎ，Ｎ−トリプロピルアンモニウム、Ｎ−ヒドロキシエチル−Ｎ，Ｎ，Ｎ−トリメチルアンモニウム、Ｎ−ヒドロキシエチル−Ｎ，Ｎ，Ｎ−トリエチルアンモニウム、Ｎ−ヒドロキシエチル−Ｎ，Ｎ，Ｎ−トリブチルアンモニウム、Ｎ−ヒドロキシエチル−Ｎ，Ｎ，Ｎ−トリプロピルアンモニウムなどが挙げられる。 Specific examples of the cation include N-methyl-N, N, N-tributylammonium, N-ethyl-N′-methylimidazolium, N-methyl-N-propylpiperidinium, N, N, N-trimethyl- N-propylammonium, N-methyl-N, N, N-tripropylammonium, N, N, N-trimethyl-N-butylammonium, N, N, N-trimethyl-N-methoxyethylammonium, N-methyl- N, N, N-tris (methoxyethyl) ammonium, N, N-dimethyl-N-butyl-N-methoxyethylammonium, N, N-dimethyl-N, N-dibutylammonium, N-methyl-N, N- Dibutyl-N-methoxyethylammonium, N, N, N-trimethyl-N-hexylammonium, N, N-diethyl-N-me Ru-N- (2-methoxyethyl) ammonium, 1-propyl-tetrahydrothiophenium, 1-butyl-tetrahydrothiophenium, 1-pentyl-tetrahydrothiophenium, 1-hexyl-tetrahydrothiophenium, glycidyltrimethyl Ammonium, N-ethylacryloyl-N, N, N-trimethylammonium, N-ethyl-N-methylmorpholinium, N, N, N-trioctylammonium, N-methyl-N, N, N-trioctylammonium N-hydroxymethyl-N, N, N-trimethylammonium, N-hydroxymethyl-N, N, N-triethylammonium, N-hydroxymethyl-N, N, N-tributylammonium, N-hydroxymethyl-N, N, N-tripropylammonium, -Hydroxyethyl-N, N, N-trimethylammonium, N-hydroxyethyl-N, N, N-triethylammonium, N-hydroxyethyl-N, N, N-tributylammonium, N-hydroxyethyl-N, N, N-tripropylammonium etc. are mentioned.
イオン液体に含まれるアニオンとしては、スルフェート（Ｒ−ＯＳＯ3 -）、スルホネート（Ｒ−ＳＯ3 -）、カルボキシレート（Ｒ−ＣＯ2 -）、ホスフェート（（ＲＯ）2Ｐ（＝Ｏ）Ｏ-）、テトラフルオロボレート（ＢＦ4 -）、テトラアルキルボレートなどの式：ＢＲ4 -で表されるボレート、ヘキサフルオロホスフェート（ＰＦ6 -）、ヘキサアルキルホスフェートなどの式：ＰＲ6 -で表されるホスフェート、イミド（Ｒ2Ｎ-）、メチド（Ｒ3Ｃ-）、硝酸イオン（ＮＯ3 -）、亜硝酸イオン（ＮＯ2 -）などであってよい。式中、Ｒは、それぞれ独立して、水素原子、ハロゲン原子（フッ素、塩素、臭素、ヨウ素）、置換または非置換の、アルキル基、アルケニル基、アルキニル基、シクロアルキル基、アリール基、アラルキル基、アリールアルキル基、アシル基、スルホニル基などであってよく、基Ｒの主鎖または環に酸素原子、窒素原子、硫黄原子などのヘテロ原子が含まれてもよく、基Ｒの炭素原子上の一部または全ての水素原子がフッ素原子で置換されていてもよい。アニオン中に複数のＲがある場合、これらのＲは互いに同じであっても異なっていてもよい。本発明においては、耐熱性が良好であることからアニオンがフッ素原子を有することが好ましく、パーフルオロアルキル基、テトラフルオロボレート基を含有することが好ましい。 Examples of anions contained in the ionic liquid include sulfate (R—OSO 3 − ), sulfonate (R—SO 3 − ), carboxylate (R—CO 2 − ), phosphate ((RO) 2 P (═O) O −. ), Tetrafluoroborate (BF 4 − ), tetraalkylborate and the like: borate represented by BR 4 − , hexafluorophosphate (PF 6 − ), hexaalkylphosphate and the like: PR 6 − It may be phosphate, imide (R 2 N − ), methide (R 3 C − ), nitrate ion (NO 3 − ), nitrite ion (NO 2 − ) or the like. In the formula, each R is independently a hydrogen atom, a halogen atom (fluorine, chlorine, bromine, iodine), a substituted or unsubstituted alkyl group, alkenyl group, alkynyl group, cycloalkyl group, aryl group, aralkyl group. , An arylalkyl group, an acyl group, a sulfonyl group, etc., and the main chain or ring of the group R may contain a heteroatom such as an oxygen atom, a nitrogen atom, a sulfur atom, etc. Some or all of the hydrogen atoms may be substituted with fluorine atoms. When there are a plurality of R in the anion, these Rs may be the same as or different from each other. In the present invention, the anion preferably has a fluorine atom because of good heat resistance, and preferably contains a perfluoroalkyl group or a tetrafluoroborate group.
パーフルオロアルキル基を含有するアニオンとして、例えば、ビス（パーフルオロアルキルスルホニル）イミド（（ＲfＳＯ2）2Ｎ-）、パーフルオロアルキルスルホネート（ＲｆＳＯ3 -）、トリス（パーフルオロアルキルスルホニル）メチド（（ＲｆＳＯ2）3Ｃ-）などが有利に使用できる（式中、Ｒｆはパーフルオロアルキル基を表す）。パーフルオロアルキル基の炭素原子数は、例えば１〜２０、１〜１２または１〜８とすることができる。ビス（パーフルオロアルキルスルホニル）イミドの具体例として、ビス（トリフルオロメタンスルホニル）イミド、ビス（ペンタフルオロエタンスルホニル）イミド、ビス（ヘプタフルオロプロパンスルホニル）イミド、ビス（ノナフルオロブタンスルホニル）イミドなどが挙げられる。パーフルオロアルキルスルホネートの具体例として、トリフルオロメタンスルホネート、ペンタフルオロエタンスルホネート、ヘプタフルオロプロパンスルホネート、ノナフルオロブタンスルホネートなどが挙げられる。トリス（パーフルオロアルキルスルホニル）メチドの具体例として、トリス（トリフルオロメタンスルホニル）メチド、トリス（ペンタフルオロエタンスルホニル）メチド、トリス（ヘプタフルオロプロパンスルホニル）メチド、トリス（ノナフルオロブタンスルホニル）メチドなどが挙げられる。
上記カチオンおよびアニオンから構成されるイオン液体として、Ｎ−メチル−Ｎ−プロピルピペリジニウムビス（トリフルオロメタンスルホニル）イミド、Ｎ−メチル−Ｎ−プロピルピペリジニウムビス（トリフルオロメタンスルホニル）イミド、Ｎ−エチル−Ｎ’−メチルイミダゾリウムビス（トリフルオロメタンスルホニル）イミド、Ｎ，Ｎ，Ｎ−トリメチル−Ｎ−ヘキシルアンモニウムビス（トリフルオロメタンスルホニル）イミド、Ｎ−メチル−Ｎ，Ｎ，Ｎ−トリブチルアンモニウムビス（トリフルオロメタンスルホニル）イミドが、耐熱性に優れかつフルオロポリマーとの相溶性が良好であることから、特に有利に使用できる。また、非着色性が求められる用途では、芳香環を含まないＮ−メチル−Ｎ−プロピルピペリジニウムビス（トリフルオロメタンスルホニル）イミド、Ｎ，Ｎ，Ｎ−トリメチル−Ｎ−ヘキシルアンモニウムビス（トリフルオロメタンスルホニル）イミド、Ｎ−メチル−Ｎ，Ｎ，Ｎ−トリブチルアンモニウムビス（トリフルオロメタンスルホニル）イミドが特に好適である。
Examples of the anion containing a perfluoroalkyl group include bis (perfluoroalkylsulfonyl) imide ((RfSO 2 ) 2 N − ), perfluoroalkyl sulfonate (RfSO 3 − ), tris (perfluoroalkylsulfonyl) methide (( RfSO 2 ) 3 C − ) and the like can be used advantageously (wherein Rf represents a perfluoroalkyl group). The number of carbon atoms of the perfluoroalkyl group can be, for example, 1 to 20, 1 to 12, or 1 to 8. Specific examples of bis (perfluoroalkylsulfonyl) imide include bis (trifluoromethanesulfonyl) imide, bis (pentafluoroethanesulfonyl) imide, bis (heptafluoropropanesulfonyl) imide, and bis (nonafluorobutanesulfonyl) imide. It is done. Specific examples of the perfluoroalkyl sulfonate include trifluoromethane sulfonate, pentafluoroethane sulfonate, heptafluoropropane sulfonate, and nonafluorobutane sulfonate. Specific examples of tris (perfluoroalkylsulfonyl) methide include tris (trifluoromethanesulfonyl) methide, tris (pentafluoroethanesulfonyl) methide, tris (heptafluoropropanesulfonyl) methide, tris (nonafluorobutanesulfonyl) methide and the like. It is done.
As the ionic liquid composed of the cation and the anion, N-methyl-N-propylpiperidinium bis (trifluoromethanesulfonyl) imide, N-methyl-N-propylpiperidinium bis (trifluoromethanesulfonyl) imide, N- Ethyl-N′-methylimidazolium bis (trifluoromethanesulfonyl) imide, N, N, N-trimethyl-N-hexylammonium bis (trifluoromethanesulfonyl) imide, N-methyl-N, N, N-tributylammonium bis ( Trifluoromethanesulfonyl) imide is particularly advantageous because it has excellent heat resistance and good compatibility with fluoropolymers. In applications that require non-coloring properties, N-methyl-N-propylpiperidinium bis (trifluoromethanesulfonyl) imide, N, N, N-trimethyl-N-hexylammonium bis (trifluoromethane) that does not contain an aromatic ring Sulfonyl) imide, N-methyl-N, N, N-tributylammonium bis (trifluoromethanesulfonyl) imide is particularly preferred.
本発明において用いるイオン液体としては、良好な導電性、耐熱性が得られることから以下の化学式（Ｉ）で表される化合物を好適に用いることができる。 As the ionic liquid used in the present invention, a compound represented by the following chemical formula (I) can be suitably used since good conductivity and heat resistance can be obtained.
上記化学式（Ｉ）において、ｍ、ｎはそれぞれ１〜５の整数であり、１〜３の整数であることが好ましく、１であることが最も好ましい。 In the above chemical formula (I), m and n are each an integer of 1 to 5, preferably an integer of 1 to 3, and most preferably 1.
上記化学式（Ｉ）において、Ｒ１〜Ｒ４は互いに同一もしくは異種の炭素原子数１〜５のアルキル基、炭素原子数１〜５のヒドロキシアルキル基、またはＲ′−Ｏ−（ＣＨ２）ｐ−で表されるアルコキシアルキル基（Ｒ′はメチル基またはエチル基を示し、ｐは１〜４の整数である。）を示し、これらＲ１、Ｒ２、Ｒ３およびＲ４のいずれか２個の基が環を形成していてもよい。炭素原子数１〜５のアルキル基としてはメチル基、エチル基、ｎ−プロピル基ｉ−プロピル基、ｎ−ブチル基、ｎ−ペンチル基などが挙げられ、炭素原子数１〜５のヒドロキシアルキル基としてはヒドロキシメチル基、ヒドロキシエチル基、ヒドロキシプロピル基、ヒドロキシブチル基、ヒドロキシペンチル基などが挙げられ、Ｒ′−Ｏ−（ＣＨ２）n−で表されるアルコキシアルキル基としては、メトキシまたはエトキシメチル基、メトキシまたはエトキシエチル基、メトキシまたはエトキシプロピル基、メトキシまたはエトキシブチル基が挙げられ、Ｒ1〜Ｒ4のいずれか２個の基が環を形成しているカチオンとしては、アジリジン環、アゼチジン環、ピロリジン環、ピペリジン環等を有する４級アンモニウムイオンが挙げられる。イオン液体は分子量の増加に伴い粘性が増す傾向があるため、前記Ｒ１〜Ｒ４は炭素原子数１〜３の置換基であることが好ましく、炭素原子数１〜２の置換基であることがより好ましい。 In the chemical formula (I), R 1 to R 4 are the same or different alkyl groups having 1 to 5 carbon atoms, hydroxyalkyl groups having 1 to 5 carbon atoms, or R′—O— (CH 2 ) p. -Represents an alkoxyalkyl group represented by — (R ′ represents a methyl group or an ethyl group, and p is an integer of 1 to 4), and any one of R 1 , R 2 , R 3 and R 4 Groups may form a ring. Examples of the alkyl group having 1 to 5 carbon atoms include a methyl group, an ethyl group, an n-propyl group, an i-propyl group, an n-butyl group, and an n-pentyl group, and a hydroxyalkyl group having 1 to 5 carbon atoms. Examples thereof include a hydroxymethyl group, a hydroxyethyl group, a hydroxypropyl group, a hydroxybutyl group, and a hydroxypentyl group. The alkoxyalkyl group represented by R′—O— (CH 2 ) n— is, for example, methoxy or ethoxy. Examples thereof include a methyl group, a methoxy or ethoxyethyl group, a methoxy or ethoxypropyl group, a methoxy or ethoxybutyl group, and any two groups of R1 to R4 form a ring such as an aziridine ring or azetidine ring. And quaternary ammonium ions having a pyrrolidine ring, a piperidine ring, and the like. Since the ionic liquid tends to increase in viscosity with an increase in molecular weight, R 1 to R 4 are preferably a substituent having 1 to 3 carbon atoms, and preferably a substituent having 1 to 2 carbon atoms. Is more preferable.
本発明のポリアリーレンスルフィド樹脂組成物において、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）とイオン液体（Ｂ）の配合量は発明の効果を損ねなければ特に限定されるものではないが、前記ポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して、前記イオン液体（Ｂ）が０．１〜２０質量部の範囲が好ましく、さらに前記イオン液体（Ｂ）が０．３〜１０質量部の範囲であることが更に好ましい。本発明は上記範囲において特に優れた機械的強度や成形品の表面及び厚み方向における導電性のばらつきを抑制でき、高温で加工を行った場合にも安定かつ均一な導電性を付与することができる。 In the polyarylene sulfide resin composition of the present invention, the blending amount of the polyarylene sulfide resin (A) and the ionic liquid (B) having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s]. Is not particularly limited as long as the effects of the invention are not impaired, but the ionic liquid (B) is preferably in the range of 0.1 to 20 parts by mass with respect to 100 parts by mass of the polyarylene sulfide resin (A). Furthermore, the ionic liquid (B) is more preferably in the range of 0.3 to 10 parts by mass. The present invention can control particularly excellent mechanical strength and variation in conductivity in the surface and thickness direction of the molded product within the above range, and can provide stable and uniform conductivity even when processed at high temperatures. .
＜カップリング剤（Ｃ）＞
本発明のポリアリーレンスルフィド樹脂組成物は、必要に応じ任意成分としてカップリング剤（Ｃ）を配合してなる。カップリング剤（Ｃ）としては、シラン系、チタン系などのカップリング剤が挙げられる。例えば、γ−グリシドキシプロピルトリメトキシシラン、γ−グリシドキシプロピルトリエトキシシラン、β−（３，４−エポキシシクロヘキシル）エチルトリメトキシシラン等のエポキシ基含有アルコキシシラン化合物、γ−イソシアナトプロピルトリメトキシシラン、γ−イソシアナトプロピルトリエトキシシラン、γ−イソシアナトプロピルメチルジメトキシシラン、γ−イソシアナトプロピルメチルジエトキシシラン、γ−イソシアナトプロピルエチルジメトキシシラン、γ−イソシアナトプロピルエチルジエトキシシラン、γ−イソシアナトプロピルトリクロロシラン等のイソシアナト基含有アルコキシシラン化合物、γ−（２−アミノエチル）アミノプロピルメチルジメトキシシラン、γ−（２−アミノエチル）アミノプロピルトリメトキシシラン、γ−アミノプロピルトリメトキシシラン等のアミノ基含有アルコキシシラン化合物、γ−ヒドロキシプロピルトリメトキシシラン、γ−ヒドロキシプロピルトリエトキシシラン等の水酸基含有アルコキシシラン化合物が挙げられる。
<Coupling agent (C)>
The polyarylene sulfide resin composition of the present invention comprises a coupling agent (C) as an optional component as necessary. Examples of the coupling agent (C) include silane-based and titanium-based coupling agents. For example, epoxy group-containing alkoxysilane compounds such as γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, β- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, γ-isocyanatopropyl Trimethoxysilane, γ-isocyanatopropyltriethoxysilane, γ-isocyanatopropylmethyldimethoxysilane, γ-isocyanatopropylmethyldiethoxysilane, γ-isocyanatopropylethyldimethoxysilane, γ-isocyanatopropylethyldiethoxysilane , Isocyanato group-containing alkoxysilane compounds such as γ-isocyanatopropyltrichlorosilane, γ- (2-aminoethyl) aminopropylmethyldimethoxysilane, γ- (2-aminoethyl) aminopropyltrimeth Shishiran, .gamma.-aminopropyl trimethoxy amino group-containing alkoxysilane compounds such as silane, .gamma.-hydroxypropyl trimethoxysilane, hydroxyl group-containing alkoxysilane compounds such as .gamma.-hydroxypropyl triethoxysilane and the like.
本発明において、前記カップリング剤（Ｃ）は必須成分ではなく、添加する場合その配合量は、本発明の効果を損ねなければ特に限定されるものではないが、優れた機械的強度やポリアリーレンスルフィド樹脂を増粘して優れた成形性を付与できる観点から、その下限値がポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して、０．０１質量部以上の範囲であることが好ましく、さらに０．１質量部以上の範囲であることがより好ましい。一方、上限値が、成形物の外観の悪化を抑制することができる点から、ポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して、５質量部以下の範囲であることが好ましく、さらに３質量部以下の範囲がより好ましく、さらに１．５質量部以下の範囲であることが最も好ましい。 In the present invention, the coupling agent (C) is not an essential component, and when added, the amount of the coupling agent is not particularly limited as long as the effects of the present invention are not impaired, but excellent mechanical strength and polyarylene. From the viewpoint of thickening the sulfide resin and imparting excellent moldability, the lower limit thereof is preferably in the range of 0.01 parts by mass or more with respect to 100 parts by mass of the polyarylene sulfide resin (A). A range of 0.1 parts by mass or more is more preferable. On the other hand, the upper limit is preferably in the range of 5 parts by mass or less with respect to 100 parts by mass of the polyarylene sulfide resin (A) from the viewpoint that deterioration of the appearance of the molded product can be suppressed, and further 3 masses. More preferred is a range of not more than 1.5 parts, and most preferred is a range of not more than 1.5 parts by mass.
＜その他成分＞
本発明は、本発明の効果を損ねない範囲で更に導電性フィラーを配合してもよい。これら導電性フィラーとしては公知の物が使用でき、例えば、ニッケル、銅、金、銀、アルミニウム、亜鉛、ニッケル、スズ、鉛、クロム、プラチナ、パラジウム、タングステン、モリブデンなどの金属材料およびこれら２種以上の合金、混合体、あるいはこれら金属の化合物で良好な導電性を有するものや、人造黒鉛、天然黒鉛、ガラス状カーボン、カーボンブラック、アセチレンブラック、ケッチェンブラック、炭素繊維、カーボンナノファイバーなどの炭素材料およびこれら２種以上の混合体、またこれら導電性フィラーをシラノール基を含有する化合物を用いて被覆した複合粒子を用いても良い。特に、銀粉、カーボンブラックは、導電性の調整を簡便に行えるため好ましい。
<Other ingredients>
In the present invention, a conductive filler may be further blended as long as the effects of the present invention are not impaired. As these conductive fillers, known ones can be used, for example, nickel, copper, gold, silver, aluminum, zinc, nickel, tin, lead, chromium, platinum, palladium, tungsten, molybdenum and other metal materials and these two kinds The above alloys, mixtures, or compounds of these metals having good conductivity, artificial graphite, natural graphite, glassy carbon, carbon black, acetylene black, ketjen black, carbon fiber, carbon nanofiber, etc. You may use the composite particle which coat | covered the carbon material and these 2 or more types of mixtures, and these electroconductive fillers using the compound containing a silanol group. In particular, silver powder and carbon black are preferable because the conductivity can be easily adjusted.
導電性フィラーの形状は、発明の効果を損ねなければ特に限定されることはなく、板状、球状、繊維状、無定形等いずれであってよい。 The shape of the conductive filler is not particularly limited as long as the effects of the invention are not impaired, and may be any of a plate shape, a spherical shape, a fiber shape, an amorphous shape, and the like.
本発明の導電性フィラーとしては、一次粒子の平均粒子径が０．０１〜１０μｍの範囲のものを用いることが好ましく、０．０１〜５μｍの範囲のものを用いることがより好ましい。この範囲の導電性フィラーは、シラノール基を含有する化合物を用いて被覆してなることが、成形時の流動性の改善効果がより大きく、流動性をより良好とすることができ、安定的に良好な導電性を奏することができる。 As the conductive filler of the present invention, those having an average primary particle size in the range of 0.01 to 10 μm are preferably used, and those having a range of 0.01 to 5 μm are more preferable. The conductive filler in this range is formed by coating with a compound containing a silanol group, and the effect of improving the fluidity during molding is greater, the fluidity can be made better, and stable. Good electrical conductivity can be achieved.
本発明のポリアリーレンスルフィド樹脂組成物における前記導電性フィラーの配合量は、本発明の効果を損ねなければ特に限定されるものではないが、優れた機械的強度や導電性を付与できる観点から、ポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して、１質量部以上の範囲であることが好ましく、さらに３質量部以上の範囲であることがより好ましく、さらに５質量部以上の範囲であることが最も好ましい。一方、成形物の外観の悪化を抑制することができる点から、ポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して、５０質量部以下の範囲であることが好ましく、さらに４０質量部以下の範囲がより好ましく、さらに３０質量部以下の範囲であることが最も好ましい。 The blending amount of the conductive filler in the polyarylene sulfide resin composition of the present invention is not particularly limited as long as the effects of the present invention are not impaired, but from the viewpoint of imparting excellent mechanical strength and conductivity, It is preferably in the range of 1 part by mass or more, more preferably in the range of 3 parts by mass or more, and further in the range of 5 parts by mass or more with respect to 100 parts by mass of the polyarylene sulfide resin (A). Is most preferred. On the other hand, from the viewpoint of suppressing deterioration of the appearance of the molded product, the range is preferably 50 parts by mass or less and more preferably 40 parts by mass or less with respect to 100 parts by mass of the polyarylene sulfide resin (A). Is more preferable, and the range of 30 parts by mass or less is most preferable.
本発明のポリアリーレンスルフィド樹脂組成物は、必要に応じ、耐衝撃性付与剤を任意成分として配合してなる。耐衝撃性付与剤としては、本発明の効果を損ねなければ特に限定されないが、例えばα−オレフィン類とビニル重合性化合物とを共重合して得られる前記熱可塑性エラストマーなどが挙げられる。前記α−オレフィン類としては、例えば、エチレン、プロピレン、ブテン−１等の炭素原子数２〜８の範囲のα−オレフィン類などが挙げられる。前記ビニル重合性化合物としては、例えば、（メタ）アクリル酸、（メタ）アクリル酸エステル等のα，β−不飽和カルボン酸類及びそのアルキルエステル類、マレイン酸、フマル酸、イタコン酸、その他の炭素原子数４〜１０の範囲の不飽和ジカルボン酸類とそのモノ及びジエステル類、その酸無水物等のα，β−不飽和ジカルボン酸及びその誘導体、グリシジル（メタ）アクリレート等が挙げられる。なお、本発明において耐衝撃性付与剤は必須成分ではないが、添加する場合、その配合量は、ポリアリーレンスルフィド樹脂１００質量部に対して１〜４０質量部の範囲であることが好ましく、５〜２０質量部の範囲であることがより好ましい。かかる範囲において、樹脂組成物が良好な耐コロナ性と成形性、特に離形性を有し、かつ成形品がエポキシ樹脂やシリコーン樹脂などの硬化性樹脂と優れた接着性を呈しつつ、さらに機械的強度、特に耐衝撃性や靱性が向上するため好ましい。 The polyarylene sulfide resin composition of the present invention comprises an impact resistance imparting agent as an optional component, if necessary. The impact resistance imparting agent is not particularly limited as long as the effects of the present invention are not impaired, and examples thereof include the thermoplastic elastomer obtained by copolymerizing α-olefins and a vinyl polymerizable compound. Examples of the α-olefins include α-olefins having 2 to 8 carbon atoms, such as ethylene, propylene, and butene-1. Examples of the vinyl polymerizable compound include α, β-unsaturated carboxylic acids such as (meth) acrylic acid and (meth) acrylic acid esters and alkyl esters thereof, maleic acid, fumaric acid, itaconic acid, and other carbons. Examples thereof include unsaturated dicarboxylic acids having 4 to 10 atoms and mono- and diesters thereof, α, β-unsaturated dicarboxylic acids such as acid anhydrides and derivatives thereof, glycidyl (meth) acrylate, and the like. In the present invention, the impact resistance imparting agent is not an essential component, but when added, the blending amount is preferably in the range of 1 to 40 parts by mass with respect to 100 parts by mass of the polyarylene sulfide resin. More preferably, it is in the range of ˜20 parts by mass. In such a range, the resin composition has good corona resistance and moldability, particularly mold release properties, and the molded product exhibits excellent adhesiveness with curable resins such as epoxy resins and silicone resins. It is preferable because the mechanical strength, particularly impact resistance and toughness are improved.
本発明のポリアリーレンスルフィド樹脂組成物は、必要に応じて繊維状および／または粒状の強化剤を任意成分として配合してなる。強化剤は、必須成分ではないものの前記ポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して４００質量部を越えない範囲で配合することが可能である。強化剤を通常は、１〜３００質量部の範囲で配合することにより強度、剛性、耐熱性、寸法安定性などのさらなる向上を図ることが可能である。 The polyarylene sulfide resin composition of the present invention is formed by blending a fibrous and / or granular reinforcing agent as an optional component, if necessary. Although the reinforcing agent is not an essential component, it can be blended in a range not exceeding 400 parts by mass with respect to 100 parts by mass of the polyarylene sulfide resin (A). Usually, it is possible to further improve the strength, rigidity, heat resistance, dimensional stability and the like by blending the reinforcing agent in the range of 1 to 300 parts by mass.
繊維状強化剤としては、ガラス繊維、シラスガラス繊維、アルミナ繊維、炭化珪素繊維、セラミック繊維、アスベスト繊維、石コウ繊維、金属繊維などの無機繊維および炭素繊維等が挙げられる。 Examples of the fibrous reinforcing agent include glass fibers, shirasu glass fibers, alumina fibers, silicon carbide fibers, ceramic fibers, asbestos fibers, stone fiber fibers, and metal fibers, carbon fibers, and the like.
粒状の強化剤としては、ワラステナイト、セリサイト、カオリン、マイカ、クレー、ベントナイト、アスベスト、タルク、アルミナシリケートなどの珪酸塩、アルミナ、塩化珪素、酸化マグネシウム、酸化ジルコニウム、酸化チタンなどの金属酸化物、炭酸カルシウム、炭酸マグネシウム、ドロマイトなどの炭酸塩、硫酸カルシウム、硫酸バリウムなどの硫酸塩、ガラス・ビーズ、窒化ホウ素、炭化珪素、シリカなどが挙げられ、これらは中空であってもよい。 Examples of granular reinforcing agents include silicates such as wollastonite, sericite, kaolin, mica, clay, bentonite, asbestos, talc, and alumina silicate, and metal oxides such as alumina, silicon chloride, magnesium oxide, zirconium oxide, and titanium oxide. And carbonates such as calcium carbonate, magnesium carbonate, and dolomite, sulfates such as calcium sulfate and barium sulfate, glass beads, boron nitride, silicon carbide, and silica. These may be hollow.
強化剤は２種以上を併用することが可能であり、必要によりシラン系、チタン系などのカップリング剤で予備処理して使用することができる。 Two or more reinforcing agents can be used in combination, and can be used after pretreatment with a coupling agent such as silane or titanium if necessary.
更に、本発明のポリアリーレンスルフィド樹脂組成物は、上記成分に加えて、さらに用途に応じて、適宜、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、ポリカーボネート樹脂、ポリフェニレンエーテル樹脂、ポリスルフォン樹脂、ポリエーテルスルフォン樹脂、ポリエーテルエーテルケトン樹脂、ポリエーテルケトン樹脂、ポリアリーレン樹脂、ポリエチレン樹脂、ポリプロピレン樹脂、ポリ四弗化エチレン樹脂、ポリ二弗化エチレン樹脂、ポリスチレン樹脂、ＡＢＳ樹脂、フェノール樹脂、ウレタン樹脂、液晶ポリマー等の合成樹脂、或いは、弗素ゴム等のエラストマーなどを任意成分として配合してなる。また、これらの樹脂は必須成分ではないが、添加する場合、その配合量は、それぞれの目的に応じて異なり、一概に規定することはできないが、ポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して０．０１〜１０００質量部の範囲で、本発明の効果を損なわないよう目的や用途に応じて適宜調整して用いればよい。 Furthermore, in addition to the above components, the polyarylene sulfide resin composition of the present invention may further comprise a polyester resin, a polyamide resin, a polyimide resin, a polyetherimide resin, a polycarbonate resin, a polyphenylene ether resin, a polysulfone, depending on the intended use. Resin, polyethersulfone resin, polyetheretherketone resin, polyetherketone resin, polyarylene resin, polyethylene resin, polypropylene resin, polytetrafluoroethylene resin, polydifluoroethylene resin, polystyrene resin, ABS resin, phenol resin Further, synthetic resin such as urethane resin and liquid crystal polymer, or elastomer such as fluorine rubber is blended as an optional component. In addition, these resins are not essential components, but when added, the blending amount differs depending on the purpose and cannot be specified unconditionally, but with respect to 100 parts by mass of the polyarylene sulfide resin (A). In the range of 0.01 to 1000 parts by mass, it may be appropriately adjusted according to the purpose and application so as not to impair the effects of the present invention.
また本発明のポリアリーレンスルフィド樹脂組成物は、その他にも離型剤、着色剤、帯電防止剤、酸化防止剤、耐熱安定剤、紫外線安定剤、紫外線吸収剤、発泡剤、難燃剤、難燃助剤、防錆剤、滑剤、結晶核剤等の公知慣用の添加剤を必要に応じ、任意成分として配合してもよい。これらの添加剤は必須成分ではないが、添加する場合、その配合量は、それぞれの目的に応じて異なり、一概に規定することはできないが、ポリアリーレンスルフィド樹脂（Ａ）１００質量部に対して０．０１〜１０００質量部の範囲で、本発明の効果を損なわないよう目的や用途に応じて適宜調整して用いればよい。 In addition, the polyarylene sulfide resin composition of the present invention includes a mold release agent, a colorant, an antistatic agent, an antioxidant, a heat stabilizer, an ultraviolet stabilizer, an ultraviolet absorber, a foaming agent, a flame retardant, and a flame retardant. You may mix | blend well-known and usual additives, such as an adjuvant, a rust preventive agent, a lubricant, and a crystal nucleating agent, as an arbitrary component as needed. These additives are not essential components, but when added, the blending amount differs depending on the purpose and cannot be specified unconditionally, but with respect to 100 parts by mass of the polyarylene sulfide resin (A). What is necessary is just to adjust suitably according to the objective and the use so that the effect of this invention may not be impaired in the range of 0.01-1000 mass parts.
＜樹脂組成物の製造＞
本発明のポリアリーレンスルフィド樹脂組成物の製造方法は特に制限なく、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）と、イオン液体（Ｂ）を必須成分として、前記ポリアリーレンスルフィド樹脂（Ａ）の融点以上で溶融混練する。
<Manufacture of resin composition>
The method for producing the polyarylene sulfide resin composition of the present invention is not particularly limited, and the polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s], an ion Using the liquid (B) as an essential component, it is melt-kneaded at a temperature equal to or higher than the melting point of the polyarylene sulfide resin (A).
より具体的には、原料として３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）、イオン液体（Ｂ）の各必須成分と、必要に応じて、カップリング剤（Ｃ）や充填剤等のその他の任意成分を、粉末、ペレット、細片など様々な形態でタンブラー、リボンブレンダー、ヘンシェルミキサー、Ｖブレンダーなどに投入しドライブレンドした後、バンバリーミキサー、ミキシングロール、単軸または２軸の押出機およびニーダーなどの公知の溶融混練機に投入し、樹脂成分の吐出量５〜５００（ｋｇ／ｈｒ）の範囲と、スクリュー回転数１００〜５００（ｒｐｍ）と、それらの比率（吐出量／スクリュー回転数）が０．０２〜２（ｋｇ／ｈｒ／ｒｐｍ）となる条件下において溶融混練する方法が挙げられる。溶融混練を行う温度としては、樹脂温度がポリアリーレンスルフィド樹脂の融点（例えば２７０〜３８０℃）以上となる温度範囲であればよく、好ましくは該融点＋１０℃以上となる温度範囲、より好ましくは融点＋１０℃〜融点＋１００℃となる温度範囲、さらに好ましくは融点＋２０〜融点＋５０℃となる温度範囲で溶融混練することができる。また、溶融混練機への各成分の添加、混合は同時に行ってもよいし、分割して行っても良い。かかる条件下で製造することによって、前記ポリアリーレンスルフィド樹脂（Ａ）をマトリックスとし、イオン液体（Ｂ）及びその他の配合成分を均一に分散させることができ、成形品表面及び厚み方向の導電性のばらつきを抑制することが可能となる。 More specifically, the polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. as a raw material in the range of 5 to 1000 [Pa · s], each essential component of the ionic liquid (B), As needed, other optional components such as coupling agents (C) and fillers were put into various forms such as powders, pellets and strips into tumblers, ribbon blenders, Henschel mixers, V blenders, etc., and dry blended. After that, it is put into a known melt kneader such as a Banbury mixer, a mixing roll, a single or twin screw extruder and a kneader, and a resin component discharge rate in the range of 5 to 500 (kg / hr) and a screw rotation speed of 100 -500 (rpm) and the melt mixing under the condition that the ratio (discharge amount / screw rotation number) is 0.02-2 (kg / hr / rpm) How to, and the like. The temperature at which the melt kneading is performed may be a temperature range in which the resin temperature is equal to or higher than the melting point of the polyarylene sulfide resin (for example, 270 to 380 ° C.), preferably the melting point + 10 ° C. or higher, more preferably the melting point. Melting and kneading can be performed in a temperature range of + 10 ° C to melting point + 100 ° C, more preferably in a temperature range of melting point +20 to melting point + 50 ° C. Moreover, the addition and mixing of each component to the melt kneader may be performed simultaneously or may be performed separately. By producing under such conditions, the polyarylene sulfide resin (A) can be used as a matrix, and the ionic liquid (B) and other compounding components can be uniformly dispersed, and the surface of the molded product and the conductive material in the thickness direction can be dispersed. Variations can be suppressed.
前記溶融混練機としては分散性や生産性の観点から二軸混練押出機が好ましく、例えば、樹脂成分の吐出量５〜５００（ｋｇ／ｈｒ）の範囲と、スクリュー回転数５０〜５００（ｒｐｍ）の範囲とを適宜調整しながら溶融混練することが好ましく、それらの比率（吐出量／スクリュー回転数）が０．０２〜５（ｋｇ／ｈｒ／ｒｐｍ）なる条件下に溶融混練することがさらに好ましい。更に、２軸押出機のトルクは最大トルクが２０〜１００（Ａ）、特に２５〜８０（Ａ）となる範囲であると、ポリアリーレンスルフィド樹脂（Ａ）をマトリックスとして、前記イオン液体（Ｂ）が均一に分散されるため好ましい。また、前記成分のうち充填剤や添加剤を添加する場合は、前記二軸混練押出機のサイドフィーダーから該押出機内に投入することが分散性の観点から好ましい。かかるサイドフィーダーの位置は、前記二軸混練押出機のスクリュー全長に対する、該押出機樹脂投入部から該サイドフィーダーまでの距離の比率が、０．１〜０．９であることが好ましい。中でも０．３〜０．７であることが特に好ましい。 The melt kneader is preferably a biaxial kneader / extruder from the viewpoint of dispersibility and productivity. For example, the resin component discharge rate is in the range of 5 to 500 kg / hr, and the screw rotation speed is 50 to 500 (rpm). It is preferable to melt-knead while appropriately adjusting the range of the above, more preferably melt-kneaded under the condition that the ratio (discharge amount / screw rotation number) is 0.02 to 5 (kg / hr / rpm). . Further, the torque of the twin-screw extruder is in the range where the maximum torque is 20 to 100 (A), particularly 25 to 80 (A), and the ionic liquid (B) using the polyarylene sulfide resin (A) as a matrix. Is preferable because it is uniformly dispersed. Moreover, when adding a filler and an additive among the said components, it is preferable from a dispersible viewpoint to throw in in this extruder from the side feeder of the said biaxial kneading extruder. The position of the side feeder is preferably such that the ratio of the distance from the extruder resin charging part to the side feeder with respect to the total screw length of the biaxial kneading extruder is 0.1 to 0.9. Especially, it is especially preferable that it is 0.3-0.7.
このように溶融混練して得られる本発明のポリアリーレンスルフィド樹脂組成物は、必須成分である３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）、イオン液体（Ｂ）、必要に応じて加える任意成分およびそれらの由来成分を配合してなる溶融混練物であり、該溶融混練後に公知の方法でペレット、チップ、顆粒、粉末等の形態に加工し、必要に応じて１００〜１５０℃の温度で予備乾燥を施した後、直接各種公知の成形法を用いて成形品へと成形されるか、これを各種成形機に供して溶融成形することにより、目的とするシート状、フィルム状など各種形状の熱可塑性樹脂成形品に成形することができる。 Thus, the polyarylene sulfide resin composition of the present invention obtained by melt-kneading is a polyarylene sulfide whose melt viscosity (V6) measured at 300 ° C., which is an essential component, is in the range of 5 to 1000 [Pa · s]. Resin (A), ionic liquid (B), an optional component added as necessary, and a melt-kneaded product obtained by blending these components, and after the melt-kneading, pellets, chips, granules, powder, etc. After being preliminarily dried at a temperature of 100 to 150 ° C. as necessary, it is directly molded into a molded product using various known molding methods or provided to various molding machines. By melt-molding, it can be molded into thermoplastic resin molded products of various shapes such as a desired sheet shape and film shape.
本発明のポリアリーレンスルフィド樹脂組成物は、射出成形、圧縮成形、コンポジット、シート、パイプなどの押出成形、引抜成形、ブロー成形、トランスファー成形など各種成形に供することが可能であるが、特に離形性にも優れるため射出成形用途に適している。射出成形にて成形する場合、各種成形条件は特に限定されず、通常一般的な方法にて成形することができる。例えば、射出成形機内で、樹脂温度がポリアリーレンスルフィド樹脂の融点以上の温度範囲、好ましくは該融点＋１０℃以上の温度範囲、より好ましくは融点＋１０℃〜融点＋１００℃の温度範囲、さらに好ましくは融点＋２０〜融点＋５０℃の温度範囲で前記ポリアリーレンスルフィド樹脂組成物を溶融する工程を経た後、樹脂吐出口よりを金型内に注入して成形すればよい。その際、金型温度も公知の温度範囲、例えば、室温（２３℃）〜３００℃の範囲、好ましくは１２０〜１８０℃に設定すればよい。 The polyarylene sulfide resin composition of the present invention can be subjected to various moldings such as injection molding, compression molding, extrusion molding of composites, sheets, pipes, pultrusion molding, blow molding, transfer molding, etc. It is suitable for injection molding because of its excellent properties. In the case of molding by injection molding, various molding conditions are not particularly limited, and can be usually molded by a general method. For example, in an injection molding machine, the resin temperature is a temperature range above the melting point of the polyarylene sulfide resin, preferably the temperature range above the melting point + 10 ° C., more preferably the temperature range from the melting point + 10 ° C. to the melting point + 100 ° C., more preferably the melting point. After passing through the step of melting the polyarylene sulfide resin composition in a temperature range of +20 to melting point + 50 ° C., the resin discharge port may be injected into the mold and molded. At that time, the mold temperature may be set to a known temperature range, for example, a room temperature (23 ° C.) to 300 ° C., preferably 120 to 180 ° C.
このようにして得られたポリアリーレンスルフィド樹脂組成物の３００℃における溶融粘度は特に制限されるものではないが、射出成形用途としては１０〜３００〔Ｐａ・ｓ〕であることが好ましく、さらにフィルムまたはシート用途としては３０〜２０００〔Ｐａ・ｓ〕のものを好適に用いることができる。 The melt viscosity at 300 ° C. of the polyarylene sulfide resin composition thus obtained is not particularly limited, but is preferably 10 to 300 [Pa · s] as an injection molding application, and further a film Or as a sheet | seat use, the thing of 30-2000 [Pa * s] can be used conveniently.
そして得られた成形品は、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）からなるマトリックス中に、イオン液体（Ｂ）が分散してなるものであって、ポリアリーレンスルフィド樹脂に均一な導電性を付与することができる。 The obtained molded product has an ionic liquid (B) in a matrix composed of a polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. of 5 to 1000 [Pa · s]. It is formed by dispersion and can impart uniform conductivity to the polyarylene sulfide resin.
＜成形品＞
本発明のポリアリーレンスルフィド樹脂組成物は、射出成形法、圧縮成形法、押出し成形法、中空成形法などの公知慣用の成形法により、様々な形状の部品・部材に成形することができ、例えば、プリンタ、コネクター、ソケット、リレー部品、コイルボビン、光ピックアップ、発振子、プリント配線板、コンピュータ関連部品、等の電気・電子部品；ＩＣトレー、ウエハーキャリヤー、等の半導体製造プロセス関連部品；ＶＴＲ、テレビ、アイロン、エアコン、ステレオ、掃除機、冷蔵庫、炊飯器、照明器具、等の家庭電気製品部品；ランプリフレクター、ランプホルダー、等の照明器具部品；コンパクトディスク、レーザディスク（登録商標）、スピーカー、等の音響製品部品；光ケーブル用フェルール、電話機部品、ファクシミリ部品、モデム、等の通信機器部品；転写ベルト、印刷ロール、分離爪、ヒータホルダー、等の複写機関連部品；燃料タンク、チューブ、インペラー、ファン、歯車、ギヤ、軸受け、モーター部品及びケース、等の機械部品；自動車用機構部品、エンジン部品、エンジンルーム内部品、電装部品、内装部品、等の自動車部品；マイクロ波調理用鍋、耐熱食器、等の調理用器具；床材、壁材などの断熱、防音用材料、梁、柱などの支持材料、屋根材、等の建築資材または土木建築用材料；航空機部品、宇宙機部品、原子炉などの放射線施設部材、海洋施設部材、洗浄用治具、光学機器部品、バルブ類、パイプ類、ノズル類、フィルター類、膜、医療用機器部品及び医療用材料、センサー類部品、医療製品、サニタリー備品、スポーツ用品、レジャー用品などが挙げられる。
<Molded product>
The polyarylene sulfide resin composition of the present invention can be molded into various shapes of parts and members by known and conventional molding methods such as injection molding, compression molding, extrusion molding, and hollow molding. , Printers, connectors, sockets, relay parts, coil bobbins, optical pickups, oscillators, printed wiring boards, computer-related parts, etc .; semiconductor manufacturing process-related parts such as IC trays, wafer carriers, VTRs, televisions Home appliance parts such as irons, air conditioners, stereos, vacuum cleaners, refrigerators, rice cookers, and luminaires; luminaire parts such as lamp reflectors and lamp holders; compact discs, laser discs (registered trademark), speakers, etc. Acoustic product parts; optical cable ferrules, telephone parts, facsimile parts Communication equipment parts such as modems; copy machine related parts such as transfer belts, printing rolls, separation claws, and heater holders; machines such as fuel tanks, tubes, impellers, fans, gears, gears, bearings, motor parts and cases Automobile parts such as automotive parts, engine parts, engine compartment parts, electrical parts, interior parts, etc .; cooking utensils such as microwave cooking pots, heat-resistant dishes, etc .; insulation for flooring, wall materials, etc. Soundproof materials, supporting materials such as beams and pillars, building materials such as roofing materials, and civil engineering materials; aircraft parts, spacecraft parts, radiation facility members such as nuclear reactors, marine facility members, cleaning jigs, optics Equipment parts, valves, pipes, nozzles, filters, membranes, medical equipment parts and medical materials, sensor parts, medical products, sanitary equipment, sports equipment, leisure And the like.
＜電子写真用転写ベルトの製造＞
冷却を行い、所望により粉砕して得たポリアリーレンスルフィド樹脂組成物のペレットは、樹脂組成物中の導電性材料の均一分散が達成され、導電性に優れた、特に、成形品の表面及び厚み方向で導電性のばらつきを抑える性能を付与可能な樹脂組成物とすることができる。
<Manufacture of electrophotographic transfer belt>
The pellets of the polyarylene sulfide resin composition obtained by cooling and pulverizing as desired achieves uniform dispersion of the conductive material in the resin composition and is excellent in conductivity, particularly the surface and thickness of the molded product. It can be set as the resin composition which can provide the performance which suppresses the dispersion | variation in electroconductivity by direction.
成形品、特にシート又はフィルムの導電性は、樹脂組成物中の前記イオン液体（Ｂ）の割合に応じて調製することができ、例えば、１０の９乗〜１１乗〔Ω／□〕とすることも可能である。 The conductivity of the molded article, particularly the sheet or film, can be prepared according to the ratio of the ionic liquid (B) in the resin composition, and is, for example, 10 9 to 11 [Ω / □]. It is also possible.
このため、シート又はフィルム状物を電子写真用転写ベルトとして用いることができる。目的とする電子写真用転写ベルトに成形するためには、３００℃で測定した溶融粘度（Ｖ６）が５〜１０００〔Ｐａ・ｓ〕の範囲であるポリアリーレンスルフィド樹脂（Ａ）と、イオン液体（Ｂ）とを配合してなるポリアリーレンスルフィド樹脂組成物をさらに成形機に供して押出成形法、射出成形法、圧縮成形法、吹込成形法、射出圧縮成形法などの公知の各種成形法に適用して、シートまたはフィルムとして得る。シートまたはフィルムの形状は特に制限されず、例えば、環状に押出成形してシームレス環形状、シート状形状を円筒に加工したもの等が挙げられる。本発明の転写ベルトはシームレス環状形状を有することが好ましい。 For this reason, a sheet or a film-like material can be used as an electrophotographic transfer belt. In order to form an intended electrophotographic transfer belt, a polyarylene sulfide resin (A) having a melt viscosity (V6) measured at 300 ° C. in the range of 5 to 1000 [Pa · s], and an ionic liquid ( The polyarylene sulfide resin composition obtained by blending with B) is further applied to a molding machine and applied to various known molding methods such as extrusion molding, injection molding, compression molding, blow molding, and injection compression molding. And obtained as a sheet or film. The shape of the sheet or film is not particularly limited, and examples thereof include a seamless ring shape obtained by extrusion molding in a ring shape and a sheet shape processed into a cylinder. The transfer belt of the present invention preferably has a seamless annular shape.
次いで、成形したベルト形状物を冷却することによって、導電性材料の分散形態が有効に維持され、導電性に優れた電子写真用転写ベルトが得られる。冷却は、ベルト形状物を室温で放置すればよい。 Next, by cooling the formed belt-shaped product, an electrophotographic transfer belt excellent in conductivity can be obtained, in which the dispersed form of the conductive material is effectively maintained. For cooling, the belt-shaped object may be left at room temperature.
なお、前記添加剤や強化剤は通常、樹脂組成物を溶融混練する際に添加、混合するが、樹脂組成物のベルト形状への成形工程でサイドフィーダーを用いて添加・混合してもよい。特に配合量が少ない添加剤は、ベルト形状への成形工程直前に添加・混合してもよい。 In addition, although the said additive and a reinforcement | strengthening agent are normally added and mixed when melt-kneading a resin composition, you may add and mix using a side feeder at the shaping | molding process to the belt shape of a resin composition. In particular, an additive with a small blending amount may be added and mixed immediately before the forming step into the belt shape.
前記の転写ベルトは、感光体上に形成されたトナー像を自己の表面に一旦、転写させた後、転写されたトナー像を紙等の記録材にさらに転写させるための中間転写ベルトであってもよいし、または紙を静電気により吸着し感光体上に形成されたトナー像をその紙に直接転写する直接転写ベルトであってもよい。 The transfer belt is an intermediate transfer belt for transferring a toner image formed on a photosensitive member to its surface once, and further transferring the transferred toner image to a recording material such as paper. Alternatively, it may be a direct transfer belt for directly adhering a toner image formed on a photosensitive member by electrostatically adsorbing the paper to the paper.
前記の転写ベルトは、前記樹脂組成物からなるベルトをそのまま用いても良いが、転写効率を高めるために、表面だけを硬くすると、本発明の効果をさらに有効に得ることができる。表面だけを硬くする方法として無機材料をコーティングする方法がよいが、その方法は特に限定されるものではない。例えば、「ゾル−ゲル法応用技術の新展開」（ＣＭＣ出版）に記載されているような塗布による方法、「薄膜材料入門」（裳華房）に記載されたＣＶＤ、ＰＶＤ、プラズマコーティングなどの物理化学的方法など、公知の方法を採用できる。表面にコーティングされる無機材料は、本発明の目的を達成できる限り特に制限されず、物性と経済性を考慮すると、Ｓｉ、Ａｌ、Ｃを含む酸化物系材料が特に好ましい。例えば、アモルファスシリカ薄膜、アモルファスアルミナ薄膜、アモルファスシリカアルミナ薄膜、アモルファスダイヤモンド薄膜などが推奨される。このようなＰＰＳよりも硬度の高い無機薄膜を本発明のベルトにコーティングすることにより、ブレードとの摩擦磨耗寿命が改善されるだけでなく、転写性も向上する。 As the transfer belt, a belt made of the resin composition may be used as it is, but the effect of the present invention can be obtained more effectively by hardening only the surface in order to increase the transfer efficiency. As a method for hardening only the surface, a method of coating an inorganic material is preferable, but the method is not particularly limited. For example, a method by coating as described in “New Development of Sol-Gel Method Application Technology” (CMC Publishing), CVD, PVD, plasma coating, etc. described in “Introduction to Thin Film Materials” (Yuhuabo) Known methods such as a physicochemical method can be employed. The inorganic material coated on the surface is not particularly limited as long as the object of the present invention can be achieved, and an oxide-based material containing Si, Al, and C is particularly preferable in view of physical properties and economy. For example, an amorphous silica thin film, an amorphous alumina thin film, an amorphous silica alumina thin film, an amorphous diamond thin film, etc. are recommended. By coating the belt of the present invention with an inorganic thin film having a hardness higher than that of PPS, not only the friction wear life with the blade is improved, but also the transferability is improved.
前記の転写ベルトは、中間転写方式の画像形成装置に用いられる転写ベルト、特に継ぎ目のないシームレスベルトに適用できる。本発明に係る転写ベルトは、現像装置に単色トナーのみを持つモノカラー画像形成装置、１つの潜像担持体に対してＹ（イエロー）、Ｍ（マゼンタ）、Ｃ（シアン）、Ｂ（ブラック）の現像器が備わり、各色の現像器ごとに潜像担持体上での現像およびトナー像の転写ベルトへの一次転写を行うサイクル方式フルカラー画像形成装置、１つの潜像担持体に対して１つの現像器が備わった各色の画像形成ユニットが直列に配置され、各色の画像形成ユニットごとに潜像担持体上での現像およびトナー像の転写ベルトへの一次転写を行うタンデム方式フルカラー画像形成装置などに適用することができる。本発明の転写ベルトを適用することにより文字の中抜けやトナーの飛び散りを抑制できる画像形成装置とすることができる。 The transfer belt can be applied to a transfer belt used in an intermediate transfer type image forming apparatus, particularly a seamless seamless belt. The transfer belt according to the present invention is a monocolor image forming apparatus having only a single color toner in the developing device, Y (yellow), M (magenta), C (cyan), B (black) for one latent image carrier. A full-color image forming apparatus that performs development on a latent image carrier and primary transfer of a toner image to a transfer belt for each color developer, one for each latent image carrier. Tandem-type full-color image forming apparatus in which image forming units for each color equipped with a developing device are arranged in series and each image forming unit performs development on a latent image carrier and primary transfer of a toner image to a transfer belt Can be applied to. By applying the transfer belt of the present invention, it is possible to provide an image forming apparatus capable of suppressing character voids and toner scattering.
以下、本発明を実施例により具体的に説明するが、本発明はこれら実施例にのみ限定されるものではない。 EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited only to these examples.
〔実施例１〜２〕
各原料を表１に記載の質量部で計量した後タンブラーで均一に混合し、配合材料とした。
[Examples 1-2]
Each raw material was weighed in parts by mass described in Table 1, and then uniformly mixed with a tumbler to obtain a blended material.
その後、株式会社日本製鋼所製ベント付き２軸押出機「ＴＥＸ−３０」に前記配合材料を投入し、樹脂成分吐出量１５ｋｇ／ｈｒ、スクリュー回転数２００（ｒｐｍ）、樹脂成分の吐出量（ｋｇ／ｈｒ）とスクリュー回転数（ｒｐｍ）との比率（吐出量／スクリュー回転数）＝０．０７５（ｋｇ／ｈｒ／ｒｐｍ）、最大トルク４０（Ａ）、設定樹脂温度３００℃で溶融混練して樹脂組成物のペレットを得た。 Thereafter, the blended material was charged into a vented twin-screw extruder “TEX-30” manufactured by Nippon Steel Works, Ltd., resin component discharge rate 15 kg / hr, screw rotation speed 200 (rpm), resin component discharge rate (kg / Hr) and screw rotation speed (rpm) ratio (discharge amount / screw rotation speed) = 0.075 (kg / hr / rpm), maximum torque 40 (A), and melt kneading at a set resin temperature of 300 ° C. A pellet of the resin composition was obtained.
得られた樹脂組成物のペレットを室温で２４時間放置した後、Ｔダイ押出機にて設定樹脂温度３００℃でフィルム化し、厚み８０μｍの導電フィルムを作製した。得られた導電フィルムは、以下の抵抗率測定、光沢測定、フィルム成形性の評価を行った。その結果を表１に示す。 The obtained resin composition pellets were allowed to stand at room temperature for 24 hours, and then formed into a film at a set resin temperature of 300 ° C. using a T-die extruder to produce a conductive film having a thickness of 80 μm. The obtained conductive film was subjected to the following resistivity measurement, gloss measurement, and film formability evaluation. The results are shown in Table 1.
〔比較例１〜２〕
実施例１におけるイオン液体の代わりとして従来導電コンパウンドに汎用されるカーボンブラックを表１に記載の質量部で配合し、実施例と同じ製造方法で導電フィルムを作成、比較例１とした。また、実施例１におけるポリアリーレンスルフィド樹脂（Ａ）の代わりとしてポリカーボネート樹脂を表１に記載の質量部で配合し、実施例と同じ製造方法で導電フィルムを作成、比較例２とした。実施例１〜２と同様に比較例１〜２の抵抗率測定、光沢測定、フィルム成形性の評価を行った。測定試験結果を表１に示す。
[Comparative Examples 1-2]
Instead of the ionic liquid in Example 1, carbon black, which has been widely used in conventional conductive compounds, was blended in the parts by mass shown in Table 1, and a conductive film was prepared by the same production method as in Example 1 to obtain Comparative Example 1. Moreover, instead of the polyarylene sulfide resin (A) in Example 1, a polycarbonate resin was blended in parts by mass shown in Table 1, and a conductive film was prepared by the same production method as in Example 1 to obtain Comparative Example 2. Similar to Examples 1 and 2, the resistivity measurement, gloss measurement, and film formability of Comparative Examples 1 and 2 were evaluated. The measurement test results are shown in Table 1.
＜表面抵抗率、体積抵抗率＞
表面抵抗率（Ω／□）及び体積抵抗率（Ω・cｍ）は、三菱化学株式会社製の抵抗測定器「ハイレスタＵＰ・ＵＲＳブローブ」を用いて２３℃、５５％ＲＨ環境下で測定した。実施例１〜２及び比較例１で作製したフィルムを、縦方向に長さ３００ｍｍにカットしたベルトをサンプルとし、該サンプルの幅方向に等ピッチで任意の３ヶ所、縦方向に任意の４カ所の合計１２ヶ所の測定点を設け、これら測定点について印加電圧１００Ｖ、１０秒後に表面抵抗率及び体積抵抗率をそれぞれ測定し、その平均値の常用対数値で示した。なお該測定サンプルは２３℃、５５％ＲＨ環境下で２４時間放置してから測定した。
<Surface resistivity, volume resistivity>
The surface resistivity (Ω / □) and the volume resistivity (Ω · cm) were measured in a 23 ° C., 55% RH environment using a resistance measuring instrument “HIRESTA UP / URS probe” manufactured by Mitsubishi Chemical Corporation. The belt produced by cutting the films produced in Examples 1 and 2 and Comparative Example 1 in the longitudinal direction to a length of 300 mm is used as a sample, and arbitrary three places at equal pitches in the width direction of the sample, and arbitrary four places in the longitudinal direction. A total of 12 measurement points were provided, and the surface resistivity and volume resistivity were measured after 10 seconds at an applied voltage of 100 V at these measurement points, and the average logarithmic value was shown. The measurement sample was measured after being left for 24 hours in an environment of 23 ° C. and 55% RH.
＜表面抵抗率平均値＞
上記１２ヶ所の測定点における表面抵抗率の平均値をρｓとした。
<Average surface resistivity>
The average value of the surface resistivity at the 12 measurement points was defined as ρs.
＜体積抵抗率平均値＞
上記１２ヶ所の測定点における体積抵抗率の平均値をρｖとした。
<Volume resistivity average value>
The average value of the volume resistivity at the 12 measurement points was defined as ρv.
＜表面抵抗率ばらつき＞
上記１２ヶ所の測定点における表面抵抗率の最大値と最小値の差をΔρsとした。
<Surface resistivity variation>
The difference between the maximum value and the minimum value of the surface resistivity at the 12 measurement points was Δρs.
＜体積抵抗率ばらつき＞
上記１２ヶ所の測定点における体積抵抗率の最大値と最小値の差をΔρvとした。
<Volume resistivity variation>
The difference between the maximum value and the minimum value of the volume resistivity at the 12 measurement points was Δρv.
＜表面抵抗率の電圧依存性＞
実施例１〜２及び比較例１で作製したフィルムに１００Ｖおよび５００Ｖの電圧を印加し、それぞれの電圧で測定された１２ヶ所の測定点における表面抵抗率平均値の差を表面抵抗率電圧依存性（Δρｓ１００−５００）とした。
<Voltage dependence of surface resistivity>
A voltage of 100 V and 500 V was applied to the films produced in Examples 1 and 2 and Comparative Example 1, and the difference in average surface resistivity at 12 measurement points measured at each voltage was determined by the surface resistivity voltage dependence. (Δρs 100-500 ).
＜体積抵抗率の電圧依存性＞
実施例１〜２及び比較例１で作製したフィルムに１００Ｖおよび５００Ｖの電圧を印加し、それぞれの電圧で測定された１２ヶ所の測定点における体積抵抗率平均値の差を体積抵抗率電圧依存性(Δρｖ１００−５００）とした。
<Voltage resistivity voltage dependency>
Voltages of 100 V and 500 V were applied to the films produced in Examples 1 and 2 and Comparative Example 1, and the difference in volume resistivity average value at 12 measurement points measured at each voltage was determined by the volume resistivity voltage dependence. (Δρv 100-500 ).
＜初期光沢測定＞
実施例１、２で得られたフィルムおよび比較例１のフィルムを、光沢計「ＶＧ２０００」（日本電色製）、入射角２０度の測定条件で光沢測定を行った。その結果をグロスで示した。
<Initial gloss measurement>
The films obtained in Examples 1 and 2 and the film of Comparative Example 1 were subjected to gloss measurement under a gloss meter “VG2000” (manufactured by Nippon Denshoku Co., Ltd.) and measurement conditions with an incident angle of 20 degrees. The results are shown in gross.
＜摩耗（ラビング）試験後の光沢測定＞
実施例１、２で得られたフィルムおよび比較例１のフィルムを用いて、太平理化工業株式会社製ラビングテスターにて、φ１７ｍｍの面積の移動擦り部に普通紙を貼付し、荷重５００g、擦り距離（片道）６０ｍｍ、擦り回数１００回の条件で擦った後、光沢値を初期光沢測定と同じ条件で測定した。
<Gloss measurement after abrasion (rubbing) test>
Using the film obtained in Examples 1 and 2 and the film of Comparative Example 1, using a rubbing tester manufactured by Taihei Rika Kogyo Co., Ltd., plain paper was affixed to a moving rubbing part having an area of φ17 mm, a load of 500 g, and a rubbing distance. (One way) After rubbing under the conditions of 60 mm and rubbing frequency of 100 times, the gloss value was measured under the same conditions as the initial gloss measurement.
＜光沢低下率＞
下記式により各フィルムの光沢低下率を評価した。
光沢低下率＝［（初期光沢−摩耗試験後の光沢）／（初期光沢）］×１００（％）
<Gloss reduction rate>
The gloss reduction rate of each film was evaluated by the following formula.
Gloss reduction rate = [(initial gloss-gloss after abrasion test) / (initial gloss)] × 100 (%)
＜フィルム成形性＞
下記式によりフィルムの成形性を評価した。
フィルム厚み精度（％）＝（フィルム両端厚みの平均値−フィルム中心部厚みの平均値 ）/フィルム中心部厚みの平均値×１００
○：５％未満 △：１０％未満 ×：１０％以上
<Film formability>
The moldability of the film was evaluated by the following formula.
Film thickness accuracy (%) = (average value of film end thickness−average value of film center thickness) / average value of film center thickness × 100
○: Less than 5% △: Less than 10% ×: 10% or more
Ｅ−２０００」
イオン液体（Ｂ）：スリーエムジャパン株式会社製「ＦＣ−４４００（商品名）、トリ-ｎ−ブチルメチルアンモニウム ビストリフルオロメタンスルホンイミド」
カーボンブラック：デンカ株式会社製「デンカブラック（登録商標）」
カップリング剤（Ｃ）：日本ユニカー社製「Ａ１８７（商品名）」（γ−グリシドキシプロピルトリメトキシシラン）
Ionic liquid (B): “FC-4400 (trade name), tri-n-butylmethylammonium bistrifluoromethanesulfonimide” manufactured by 3M Japan Ltd.
Carbon Black: “Denka Black (registered trademark)” manufactured by Denka Corporation
Coupling agent (C): “A187 (trade name)” (γ-glycidoxypropyltrimethoxysilane) manufactured by Nihon Unicar Company
Claims (7)
で表される化合物である請求項１に記載のポリアリーレンスルフィド樹脂組成物。 The ionic liquid (B) has the following chemical formula (I)
The polyarylene sulfide resin composition according to claim 1, which is a compound represented by the formula:
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| JP2013076081A (en) * | 1999-10-06 | 2013-04-25 | Three M Innovative Properties Co | Antistatic composition, and manufacturing method and use thereof |
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