JPS63251449A - Heat-resistant thermoplastic resin composition - Google Patents
Heat-resistant thermoplastic resin compositionInfo
- Publication number
- JPS63251449A JPS63251449A JP62083003A JP8300387A JPS63251449A JP S63251449 A JPS63251449 A JP S63251449A JP 62083003 A JP62083003 A JP 62083003A JP 8300387 A JP8300387 A JP 8300387A JP S63251449 A JPS63251449 A JP S63251449A
- Authority
- JP
- Japan
- Prior art keywords
- weight
- post
- resin
- vinyl chloride
- chlorinated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011342 resin composition Substances 0.000 title claims abstract description 11
- 229920005992 thermoplastic resin Polymers 0.000 title claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 54
- 239000011347 resin Substances 0.000 claims abstract description 54
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 26
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000460 chlorine Substances 0.000 claims abstract description 17
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 11
- 229920000800 acrylic rubber Polymers 0.000 claims abstract description 7
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 7
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 14
- 239000004609 Impact Modifier Substances 0.000 claims description 10
- 239000004709 Chlorinated polyethylene Substances 0.000 claims description 6
- 239000012943 hotmelt Substances 0.000 claims description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 2
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 claims 1
- WWNGFHNQODFIEX-UHFFFAOYSA-N buta-1,3-diene;methyl 2-methylprop-2-enoate;styrene Chemical compound C=CC=C.COC(=O)C(C)=C.C=CC1=CC=CC=C1 WWNGFHNQODFIEX-UHFFFAOYSA-N 0.000 claims 1
- 239000005038 ethylene vinyl acetate Substances 0.000 claims 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 11
- -1 polyethylenes Polymers 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 8
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 abstract description 7
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 abstract description 6
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004698 Polyethylene Substances 0.000 abstract description 4
- 229920000573 polyethylene Polymers 0.000 abstract description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract description 3
- 239000005977 Ethylene Substances 0.000 abstract description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 16
- 150000001875 compounds Chemical class 0.000 description 15
- 230000000704 physical effect Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000000178 monomer Substances 0.000 description 7
- 239000003381 stabilizer Substances 0.000 description 6
- 239000004801 Chlorinated PVC Substances 0.000 description 5
- 229920000457 chlorinated polyvinyl chloride Polymers 0.000 description 5
- 239000001993 wax Substances 0.000 description 5
- 229920000297 Rayon Polymers 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 239000002964 rayon Substances 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000002459 sustained effect Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 2
- LUZSPGQEISANPO-UHFFFAOYSA-N butyltin Chemical compound CCCC[Sn] LUZSPGQEISANPO-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- UQLDLKMNUJERMK-UHFFFAOYSA-L di(octadecanoyloxy)lead Chemical compound [Pb+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O UQLDLKMNUJERMK-UHFFFAOYSA-L 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- OCWMFVJKFWXKNZ-UHFFFAOYSA-L lead(2+);oxygen(2-);sulfate Chemical compound [O-2].[O-2].[O-2].[Pb+2].[Pb+2].[Pb+2].[Pb+2].[O-]S([O-])(=O)=O OCWMFVJKFWXKNZ-UHFFFAOYSA-L 0.000 description 2
- ZQBAKBUEJOMQEX-UHFFFAOYSA-N phenyl salicylate Chemical compound OC1=CC=CC=C1C(=O)OC1=CC=CC=C1 ZQBAKBUEJOMQEX-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- URJITOLRUFWZLN-DCVDYEDCSA-H (Z)-but-2-enedioate octyltin(3+) Chemical compound [O-]C(=O)\C=C/C([O-])=O.[O-]C(=O)\C=C/C([O-])=O.[O-]C(=O)\C=C/C([O-])=O.CCCCCCCC[Sn+3].CCCCCCCC[Sn+3] URJITOLRUFWZLN-DCVDYEDCSA-H 0.000 description 1
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- XXCVIFJHBFNFBO-UHFFFAOYSA-N 1-ethenoxyoctane Chemical compound CCCCCCCCOC=C XXCVIFJHBFNFBO-UHFFFAOYSA-N 0.000 description 1
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- NMAGCVWUISAHAP-UHFFFAOYSA-N 3,5-ditert-butyl-2-(2,4-ditert-butylphenyl)-4-hydroxybenzoic acid Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1C1=C(C(O)=O)C=C(C(C)(C)C)C(O)=C1C(C)(C)C NMAGCVWUISAHAP-UHFFFAOYSA-N 0.000 description 1
- 125000005274 4-hydroxybenzoic acid group Chemical class 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229920003314 Elvaloy® Polymers 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- NQSMEZJWJJVYOI-UHFFFAOYSA-N Methyl 2-benzoylbenzoate Chemical compound COC(=O)C1=CC=CC=C1C(=O)C1=CC=CC=C1 NQSMEZJWJJVYOI-UHFFFAOYSA-N 0.000 description 1
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical compound C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 description 1
- KEQFTVQCIQJIQW-UHFFFAOYSA-N N-Phenyl-2-naphthylamine Chemical compound C=1C=C2C=CC=CC2=CC=1NC1=CC=CC=C1 KEQFTVQCIQJIQW-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical class C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- FKXJWELJXMKBDI-UHFFFAOYSA-K [butyl-di(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(OC(=O)CCCCCCCCCCC)OC(=O)CCCCCCCCCCC FKXJWELJXMKBDI-UHFFFAOYSA-K 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 150000008360 acrylonitriles Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229940111121 antirheumatic drug quinolines Drugs 0.000 description 1
- 239000000981 basic dye Substances 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- 150000008366 benzophenones Chemical class 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- INLLPKCGLOXCIV-UHFFFAOYSA-N bromoethene Chemical compound BrC=C INLLPKCGLOXCIV-UHFFFAOYSA-N 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- GWOWVOYJLHSRJJ-UHFFFAOYSA-L cadmium stearate Chemical compound [Cd+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O GWOWVOYJLHSRJJ-UHFFFAOYSA-L 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- JBSLOWBPDRZSMB-BQYQJAHWSA-N dibutyl (e)-but-2-enedioate Chemical compound CCCCOC(=O)\C=C\C(=O)OCCCC JBSLOWBPDRZSMB-BQYQJAHWSA-N 0.000 description 1
- IEPRKVQEAMIZSS-AATRIKPKSA-N diethyl fumarate Chemical compound CCOC(=O)\C=C\C(=O)OCC IEPRKVQEAMIZSS-AATRIKPKSA-N 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- GLVVKKSPKXTQRB-UHFFFAOYSA-N ethenyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC=C GLVVKKSPKXTQRB-UHFFFAOYSA-N 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000010559 graft polymerization reaction Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UMKARVFXJJITLN-UHFFFAOYSA-N lead;phosphorous acid Chemical compound [Pb].OP(O)O UMKARVFXJJITLN-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229940049920 malate Drugs 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N malic acid Chemical compound OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000005397 methacrylic acid ester group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 125000000018 nitroso group Chemical group N(=O)* 0.000 description 1
- ZMHZSHHZIKJFIR-UHFFFAOYSA-N octyltin Chemical compound CCCCCCCC[Sn] ZMHZSHHZIKJFIR-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 229960000969 phenyl salicylate Drugs 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003248 quinolines Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229960001860 salicylate Drugs 0.000 description 1
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は易加工性の耐熱性熱可塑性樹脂組成物に関する
ものである。さらに詳しくいえば、本発明は、特に高温
薬液用の容器やタンク、配管、あるいは温廃水用下水配
管、電カケープル保護管などに好適な、優れた加工適性
を有し、かつ耐衝撃性、耐熱性、耐薬品性などの物性に
関しバランスのとれた成形品を与える熱可塑性樹脂組成
物に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to an easily processable heat-resistant thermoplastic resin composition. More specifically, the present invention has excellent processing suitability and is particularly suitable for containers, tanks, and piping for high-temperature chemical solutions, sewage piping for hot waste water, power cable protection pipes, etc., and has shock resistance and heat resistance. The present invention relates to a thermoplastic resin composition that provides molded products with well-balanced physical properties such as hardness and chemical resistance.
従来の技術
後塩素化塩化ビニル系樹脂は、耐薬品性、耐候性、耐燃
性に優れ、かつ、通常の塩化ビニル樹脂に比べて、はる
かに良好な耐熱性を有することが知られている。Background of the Invention Chlorinated vinyl chloride resins are known to have excellent chemical resistance, weather resistance, and flame resistance, and to have much better heat resistance than ordinary vinyl chloride resins.
しかしながら、この後塩素化塩化ビニル系樹脂は、塩化
ビニル樹脂と同様に耐衝撃性が低い上に、溶融粘度が高
く加工しにくいという欠点を有している。However, like vinyl chloride resins, chlorinated vinyl chloride resins have the disadvantages of low impact resistance, high melt viscosity, and difficulty in processing.
したがって、高温薬液用の容器やタンク、配管、あるい
は温廃水用下水配管、電カケープル保護管などの材料と
して、該後塩素化塩化ビニル樹脂を用いる場合には、そ
のままでは使用できないので、該樹脂に種々の改質剤を
配合して、前記欠点を改良することが必要とされている
。Therefore, when using post-chlorinated vinyl chloride resin as a material for containers, tanks, piping for high-temperature chemical solutions, sewage piping for hot waste water, electrical cable protection pipes, etc., it cannot be used as is, so the resin There is a need to improve the above drawbacks by incorporating various modifiers.
そして、このような改質剤を含むものとして、これまで
後塩素化塩化ビニル樹脂に対し、特定量の塩素化ポリオ
レフィンを配合したものや(特公昭38−12175号
公報)、アクリル酸アルキルエステルとスチレンとメチ
ルメタクリレートとを共重合して得られた多成分系樹脂
を配合したもの(特公昭53−18230号公報)など
が提案されているが、まだ加工性や耐衝撃性の改善は十
分に達成されていないのが現状である。So far, there have been products containing such modifiers, such as those in which a specific amount of chlorinated polyolefin is blended with post-chlorinated vinyl chloride resin (Japanese Patent Publication No. 38-12175), and those containing acrylic acid alkyl esters. Compounds of multi-component resins obtained by copolymerizing styrene and methyl methacrylate have been proposed (Japanese Patent Publication No. 18230/1983), but improvements in processability and impact resistance have not yet been achieved. The current situation is that this has not been achieved.
発明が解決しようとする問題点
本発明は、このような事情のもとで、耐熱性、耐薬品性
、耐候性、耐燃性に優れ、しかも、良好な耐衝撃性及び
加工性を有する、後塩素化ビニル系樹脂を主体とした熱
可塑性樹脂組成物を提供することを目的としてなされた
ものである。Problems to be Solved by the Invention Under these circumstances, the present invention provides a material that has excellent heat resistance, chemical resistance, weather resistance, and flame resistance, as well as good impact resistance and processability. The purpose of this invention is to provide a thermoplastic resin composition mainly composed of chlorinated vinyl resin.
問題点を解決するための手段
本発明者ら、後塩素化塩化ビニル系樹脂について、その
耐衝撃性及び加工性を改善するため鋭意研究を重ねた結
果、塩素含有量が特定の範囲にある後塩素化塩化ビニル
系樹脂に対して、耐衝撃性改良剤を所定の割合で配合す
ることによシ、前記の目的を達成しうることを見い出し
、この知見に基づいて本発明を完成するに至った。Means for Solving the Problems The present inventors have conducted intensive research on post-chlorinated vinyl chloride resins in order to improve their impact resistance and processability. We have discovered that the above object can be achieved by blending an impact modifier in a predetermined ratio with a chlorinated vinyl chloride resin, and based on this knowledge, we have completed the present invention. Ta.
すなわち、本発明は、(A)平均塩素含有量が60重量
係以上64重量係未満の後塩素化塩化ビニル系樹脂10
0重量部に対して、(B)耐衝撃性改良剤2〜10重量
部を配合して成る、良好な加工性をもつ耐熱性熱可塑性
樹脂組成物を提供するものである。That is, the present invention provides (A) a post-chlorinated vinyl chloride resin with an average chlorine content of 60 parts by weight or more and less than 64 parts by weight.
The object of the present invention is to provide a heat-resistant thermoplastic resin composition having good processability, which contains 2 to 10 parts by weight of the impact modifier (B) per 0 parts by weight.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明組成物においては、(A)成分として後塩素化塩
化ビニル系樹脂が用いられるが、この後塩素化塩化ビニ
ル系樹脂は、平均塩素含有量60重量多重上64重量%
未満のものであることが必要である。このようなものは
、公知の方法、例えば塩化ビニル系樹脂粉末を気相中又
は水中に懸濁した状態で塩素化する方法において、塩素
化条件を適当に調節することにより製造することができ
る。In the composition of the present invention, a post-chlorinated vinyl chloride resin is used as the component (A), and the post-chlorinated vinyl chloride resin has an average chlorine content of 60% by weight and 64% by weight.
It must be less than Such a product can be produced by appropriately adjusting the chlorination conditions in a known method, for example, a method in which vinyl chloride resin powder is chlorinated in a gas phase or suspended in water.
この平均塩素含有量が60重量%未満のものでは、十分
な耐熱性を有するものが得られないし、64重量係以上
のものでは溶融粘度が高く、加工性に劣る」二に、得ら
れる成形品の耐衝撃性が低下する傾向がある。また、該
後塩素化塩化ビニル系樹脂ノJISK−6721に従っ
て測定したニトロベンゼン法による固有粘度は、組成物
の加工性及び成形品の耐衝撃性をよくするために、0゜
27〜0.44の範囲にあることが好ましい。If the average chlorine content is less than 60% by weight, it will not be possible to obtain a product with sufficient heat resistance, and if it is more than 64% by weight, the melt viscosity will be high and the processability will be poor. impact resistance tends to decrease. In addition, the intrinsic viscosity of the post-chlorinated vinyl chloride resin measured by the nitrobenzene method according to JISK-6721 is 0°27 to 0.44 in order to improve the processability of the composition and the impact resistance of the molded product. Preferably within this range.
この後塩素化塩化ビニル系樹脂の製造に用いられる塩化
ビニル系樹脂は、塩化ビニル単独重合体であってもよい
し、塩化ビニルと共重合可能な他のモノマーとの塩化ビ
ニル系共重合体であってもよいが、共重合体を用いる場
合には、共重合可能な他のモノマーの含有量は、塩化ビ
ニル単位100重量部に対し、15重量部以下、好まし
くは6重量部以下であるのがよい。この共重合可能な他
のモノマーとしては、例えば酢酸ビニル、プロピオン酸
ビニル、ラウリル酸ビニルなどのビニルエステル類、メ
チルアクリレート、エチルアクリレート、ブチルアクリ
レートなどのアクリル酸エステル類、メチルメタクリレ
ート、エチルメタクリレートなどのメタクリル酸エステ
ル類、ジプチルマレート、ジエチルマレ−ドナどのマレ
イン酸エステル類、ジブチルフマレート、ジエチルフマ
レートなどのフラール酸エステル類、ビニルメチルエー
テル、ビニルブチルエーテル、ビニルオクチルエーテル
などのビニルエーテル類、アクリロニトリル、メタクリ
レートリルなどのシアン化ビニル類、エチレン、プロピ
レン、n−ブテンなどのオレフィン類、塩化ビニリデン
、臭化ビニルなどの塩化ビニル以外のハロゲン化ビニリ
デン類又はハロゲン化ビニル類などを挙げることができ
る。The vinyl chloride resin used in the subsequent production of the chlorinated vinyl chloride resin may be a vinyl chloride homopolymer or a vinyl chloride copolymer with other monomers that can be copolymerized with vinyl chloride. However, when using a copolymer, the content of other copolymerizable monomers is 15 parts by weight or less, preferably 6 parts by weight or less, based on 100 parts by weight of vinyl chloride units. Good. Examples of other copolymerizable monomers include vinyl esters such as vinyl acetate, vinyl propionate, and vinyl laurate; acrylic esters such as methyl acrylate, ethyl acrylate, and butyl acrylate; and methyl methacrylate and ethyl methacrylate. Methacrylic acid esters, maleic esters such as diptyl maleate and diethyl maledna, fullal acid esters such as dibutyl fumarate and diethyl fumarate, vinyl ethers such as vinyl methyl ether, vinyl butyl ether and vinyl octyl ether, acrylonitrile, methacrylate trile, etc. Examples include vinyl cyanides, olefins such as ethylene, propylene, and n-butene, vinylidene halides other than vinyl chloride, such as vinylidene chloride, and vinyl bromide, and vinyl halides.
本発明組成物において(B)成分として用いられる耐衝
撃性改良剤としては、多成分アクリルゴム系樹脂、後塩
素化ポリエチレン、メチルメタクリジート°フタジエン
°スチレン系樹脂、エチレン・酢酸ビニル系樹脂などが
ある。この中の多成分アクリルゴム系樹脂としては、例
えばアクリル酸エステルを主体とする共重合ゴムに、メ
チルメタクリレート、スチレン、アクリロニトリルなど
の単量体をグラフト重合した多成分系樹脂を挙げること
ができる。この多成分系樹脂は、公知の方法、例えばア
ルキル基の炭素数が2〜8のアクリル酸アルギルエステ
ルに、共重合可能なモノビニリチン化合物及び多官能性
架橋剤を反応させて、まずゴム状共重合体の水性分散液
を調製し、次いで、このゴム状共重合体20〜80重量
部に、アルキル基の炭素数が1〜4のメタクリル酸アル
キルエステル、ビニル芳香族化合物、不飽和ニトリル及
びこれらの単量体と共重合可能なモノビニリデン基を含
む単量体の全部又は2〜6種から成るグラノド用単量体
混合物80〜20重量部をグラフト重合する、といった
方法によシ製造することができる。Impact modifiers used as component (B) in the composition of the present invention include multi-component acrylic rubber resins, post-chlorinated polyethylene, methyl methacrylate/phtadiene/styrene resins, and ethylene/vinyl acetate resins. be. Among these, the multicomponent acrylic rubber resin includes, for example, a multicomponent resin obtained by graft-polymerizing monomers such as methyl methacrylate, styrene, and acrylonitrile to a copolymer rubber mainly composed of acrylic acid ester. This multi-component resin is produced by a known method, for example, by reacting an acrylic acid argyl ester having an alkyl group with 2 to 8 carbon atoms with a copolymerizable monovinyritine compound and a polyfunctional crosslinking agent, and first producing a rubber-like resin. An aqueous dispersion of the polymer is prepared, and then, to 20 to 80 parts by weight of this rubbery copolymer, a methacrylic acid alkyl ester whose alkyl group has 1 to 4 carbon atoms, a vinyl aromatic compound, an unsaturated nitrile, and these are added. Produced by a method such as graft polymerization of 80 to 20 parts by weight of a monomer mixture for granod consisting of all or 2 to 6 monomers containing a monovinylidene group copolymerizable with the monomer of Can be done.
このような多成分アクリルゴム系樹脂の市販品としては
、例えばクレハHIA−15、HIA−28(具現化学
(株)製、商品名〕、カネエースFM(鐘淵化学((ト
)製、商品名〕、メタプレンW −300、W−529
〔三菱レーヨン(掬製、商品名〕などがある。Commercial products of such multi-component acrylic rubber resins include, for example, Kureha HIA-15, HIA-28 (manufactured by Gugen Kagaku Co., Ltd., trade name), Kane Ace FM (manufactured by Kanebuchi Chemical Co., Ltd., trade name). ], Metaprene W-300, W-529
[Mitsubishi Rayon (made by scooping, product name]) etc.
また、後塩素化ポリエチレンとしては、公知のものの中
から適宜選択して用いることができるが特に塩素含量2
0〜450〜45重量部くは60〜400〜40重量部
あり、かつ非結晶性のものが適肖である。このような後
塩素化ポリエチレンの市販品としては、例えばエラスレ
ン301A。In addition, as the post-chlorinated polyethylene, it is possible to appropriately select and use from known ones, but in particular, the chlorine content is 2.
Suitable materials include 0 to 450 to 45 parts by weight or 60 to 400 to 40 parts by weight and are amorphous. A commercially available product of such post-chlorinated polyethylene is, for example, Elasrene 301A.
351A、 401A (昭和電工(株)製、商品名〕
、グイソラックH−j35 (大阪曹達(御製、商品名
〕、CPE−3614,3615(ダウケミカル社製、
商品名)などがある。351A, 401A (manufactured by Showa Denko K.K., product name)
, Guisolac H-j35 (manufactured by Osaka Soda, trade name), CPE-3614, 3615 (manufactured by Dow Chemical Company,
product name) etc.
また、メチルメタクリジート°ブタジェン°スチレン系
樹脂としては、公知の方法、例えばブタジェンを主成分
とするゴムに、メチルメタクリレート、スチレンなどを
グラフト重合する方法によって得られる多成分系樹脂(
MBS系樹脂)などを用いることができる。このような
MBS系樹脂の市販品としては、例えばメタプレンC−
223(三菱レーヨン(株)製、商品名〕、スレン・B
TA−111Nx C具現化学(株)製、商品名〕、カ
ネ力エースB−56〔鐘淵化学(株)製、商品名〕など
がある。In addition, the methyl methacrylate/butadiene/styrene resin is a multicomponent resin obtained by a known method, such as a method in which methyl methacrylate, styrene, etc. are graft-polymerized onto a rubber whose main component is butadiene.
MBS resin) or the like can be used. Commercially available MBS resins include, for example, Metaprene C-
223 (manufactured by Mitsubishi Rayon Co., Ltd., product name), Suren B
Examples include TA-111Nx C (manufactured by Gugen Kagaku Co., Ltd., trade name) and Kanerikyo Ace B-56 (manufactured by Kanefuchi Kagaku Co., Ltd., trade name).
さらに、エチレン・酢酸ビニル系樹脂(EVA系樹脂)
としては、酢酸ビニル単位18〜40モル係を含有する
ものが好適である。このようなものの市販品としては、
例えばエバフレックス250、エバフレックスIM12
、エルバロイ867.868〔以上三井ポリケミカル
(掬製、商品名〕などがある。Furthermore, ethylene/vinyl acetate resin (EVA resin)
As such, those containing 18 to 40 moles of vinyl acetate units are suitable. Commercially available products such as these include:
For example, Evaflex 250, Evaflex IM12
, Elvaloy 867, 868 [Mitsui Polychemical (manufactured by Kiki, trade name)], etc.
これらの耐衝撃性改良剤は、1種用いてもよいし、2種
以上を組み合わせて用いてもよく、またその配合量は、
(A)成分の後塩素化塩化ビニル系樹脂100重量部に
対し、2〜10重量部の範囲で選ばれる。この量が2重
量部未満では耐衝撃性及び加工性の改良効果が十分に発
揮されず、一方10重量部を超えると耐熱性及び機械的
強度が低下する。耐衝撃性改良剤として、多成分アクリ
ルゴム系樹脂や後塩素化ポリエチレンを用いる場合には
、その配合量は、6〜10重量部の範囲にあることが好
ましい。These impact resistance modifiers may be used alone or in combination of two or more, and the blending amount is as follows:
The amount is selected in the range of 2 to 10 parts by weight based on 100 parts by weight of the post-chlorinated vinyl chloride resin of component (A). If this amount is less than 2 parts by weight, the effect of improving impact resistance and processability will not be sufficiently exhibited, while if it exceeds 10 parts by weight, heat resistance and mechanical strength will decrease. When a multi-component acrylic rubber resin or post-chlorinated polyethylene is used as the impact modifier, the amount thereof is preferably in the range of 6 to 10 parts by weight.
本発明組成物には、必要に応じ各種添加剤、例えば安定
剤、滑剤、酸化防止剤、充てん剤、紫外線吸収剤、着色
剤などを添加することができる。Various additives such as stabilizers, lubricants, antioxidants, fillers, ultraviolet absorbers, colorants, etc. can be added to the composition of the present invention, if necessary.
該安定剤としては、例えば三塩基性硫酸鉛、二塩基性亜
リン酸鉛などの鉛系安定剤、ブチルスズマレート、ブチ
ルスズラウレート、ブチルスズメルカプチド、オクチル
スズマレート、オクチルスズメルカプチド、メチルスズ
メルカプチドなどのスズ系安定剤などが挙げられ、また
、滑剤としては、例えばステアリン酸鉛、ステアリン酸
カドミウム、ステアリン酸亜鉛、ステアリン酸カルシウ
ムなどの金属セッケン、パラフィンワックス、マイクロ
クリスタルワラカス、ポリエチレンワラカス、脂肪酸、
脂肪酸アミド、脂肪酸エステル、脂肪族ケトン、脂肪族
アルコール、脂肪酸の部分エステルワックスなどが、酸
化防止剤としては、例えばフェニル−α−ナフチルアミ
ン、フェニル−β−ナフチルアミン、アルドール−α−
ナノチルアミンなどのナフチルアミン系、p−インプロ
ポキシ−ジフェニルアミン、NIN′−ジフェニル−プ
ロピレンジアミンなどのジフェニルアミンL 2,2
.4−トリメチル−1,2−ジヒドロキノンの重合物、
6−ニトキシー2.2.4−トリメチル−1,2−ジヒ
ドロキノリンなどのキノリン系、1−オキシ−6−メチ
ル−4−イソプロピルベンゼン、2,6−ジー第三−ブ
チル−4−メチルフェノールなどのモノフェノール系、
4.4’−ジヒドロキシジフェニル、ヒンダードビスフ
ェノール、トリス−(2−メチル−4−ヒドロキシ−5
−第三−ブチルフェニル)ブタンなどのポリフェノール
系、4−4’−チオビス−(6−第三−プチル−6−メ
チルフェノール)などのチオビスフェノール系などが、
充てん剤としては、例えば炭酸カルシウム、ケイ酸アル
ミニウム、水酸化アルミニウム、炭酸マグネシウム、水
酸化マグネシウム、ケイソウ土、木粉、タルク、シリカ
、マイカなどが、紫外線吸収剤としては、例えばフェニ
ルサリシレート、p−オクテルフェニルサリシレートな
どのサリチル酸誘導体、2,4−ジヒドロキシベンゾフ
ェノン、2−ヒドロ+1y−4−メトキシベンゾフェノ
ンなどのベンゾフェノン系、2−(2’−ヒドロキシ−
5′−メチル−フェニル)ペンツトリアゾール、2−(
2’−ヒドロキシ−31,51−ジー第三−プチル−フ
ェニル)ベンゾトリアゾールなどのトリアゾール系、レ
ゾルシノール・モノベンゾニー)、2.4−ジー第三−
プチルフェニル−3,5−ジー第三−プチル−4−ヒド
ロキシベンゾエート、o−ベンゾイル安息香酸メチルな
どが、着色剤としては、例えば酸化チタン、鉛白、リト
ポン、パライト、カーボンブラック、カドミウムレッド
、べんがら、銀朱、カドミウムイエローなどの無機系顔
料、アゾ系顔料、ニトロソ顔料、ニトロ顔料、塩基性染
料レーキ、フタロシアニン顔料などが挙げられる。Examples of the stabilizer include lead-based stabilizers such as tribasic lead sulfate and dibasic lead phosphite, butyl tin malate, butyl tin laurate, butyl tin mercaptide, octyl tin maleate, octyl tin mercaptide, and methyl. Examples include tin-based stabilizers such as tin mercaptide, and examples of lubricants include metal soaps such as lead stearate, cadmium stearate, zinc stearate, and calcium stearate, paraffin wax, microcrystal waracas, polyethylene waracas, fatty acid,
Fatty acid amides, fatty acid esters, aliphatic ketones, fatty alcohols, fatty acid partial ester waxes, etc. are used as antioxidants, such as phenyl-α-naphthylamine, phenyl-β-naphthylamine, aldol-α-
Naphthylamine type such as nanothylamine, diphenylamine L2,2 such as p-impropoxy-diphenylamine, NIN'-diphenyl-propylene diamine, etc.
.. 4-trimethyl-1,2-dihydroquinone polymer,
Quinolines such as 6-nitoxy2.2.4-trimethyl-1,2-dihydroquinoline, 1-oxy-6-methyl-4-isopropylbenzene, 2,6-di-tert-butyl-4-methylphenol, etc. monophenolics,
4.4'-dihydroxydiphenyl, hindered bisphenol, tris-(2-methyl-4-hydroxy-5
-Polyphenols such as -tert-butylphenyl)butane, thiobisphenols such as 4-4'-thiobis-(6-tert-butyl-6-methylphenol), etc.
Examples of fillers include calcium carbonate, aluminum silicate, aluminum hydroxide, magnesium carbonate, magnesium hydroxide, diatomaceous earth, wood flour, talc, silica, mica, etc.; examples of ultraviolet absorbers include phenyl salicylate, p- Salicylic acid derivatives such as octerphenyl salicylate, benzophenones such as 2,4-dihydroxybenzophenone, 2-hydro+1y-4-methoxybenzophenone, 2-(2'-hydroxy-
5'-Methyl-phenyl)penztriazole, 2-(
Triazoles such as 2'-hydroxy-31,51-di-tertiary-butyl-phenyl)benzotriazole, resorcinol monobenzony), 2,4-di-tertiary-
Butylphenyl-3,5-di-tert-butyl-4-hydroxybenzoate, methyl o-benzoylbenzoate, etc., and examples of coloring agents include titanium oxide, lead white, lithopone, pallite, carbon black, cadmium red, red iron. Examples include inorganic pigments such as , silver vermillion, and cadmium yellow, azo pigments, nitroso pigments, nitro pigments, basic dye lakes, and phthalocyanine pigments.
これらの添加剤の配合量については、本発明の目的をそ
こなわない範囲で任意に選択することができるが、通常
前記の(A)成分と(B)成分との合計重量に基づき、
安定剤は5重量%以下、滑剤は0・5〜5重量%、酸化
防止剤は2重量%以下、充てん剤は100重量%以下紫
外線吸収剤は2重量%以下、着色剤は6重量%以下の範
囲で選ばれる。The amount of these additives can be arbitrarily selected within a range that does not impair the purpose of the present invention, but usually based on the total weight of components (A) and (B),
Stabilizer: 5% by weight or less, lubricant: 0.5 to 5% by weight, antioxidant: 2% by weight or less, filler: 100% by weight or less, ultraviolet absorber: 2% by weight or less, colorant: 6% by weight or less selected within the range.
本発明組成物は、前記の(A)成分、(B)成分及び必
要に応じて用いられる各種添加剤を、例えばヘンシェル
ミキサーやスーパーミキサーなどの高速ミキサー、リボ
ンブレンダー、バンバリーミキサ−1連続ニーグー、ミ
キシングロール、ライカイキなどの混合機に投入し、適
当な温度で均一に混合することにより調製することがで
きる。The composition of the present invention can be prepared by mixing the above-mentioned (A) component, (B) component, and various additives used as necessary with a high-speed mixer such as a Henschel mixer or a super mixer, a ribbon blender, a Banbury mixer-1 continuous mixer, etc. It can be prepared by putting it into a mixer such as a mixing roll or a laikaiki and mixing it uniformly at an appropriate temperature.
このようにして調製された本発明の熱可塑性樹脂組成物
は、加工性の点からその熱溶融粘度が319・m以下の
ものが好適である。The thermoplastic resin composition of the present invention prepared in this manner preferably has a hot melt viscosity of 319 m or less from the viewpoint of processability.
発明の効果
本発明の熱可塑性樹脂組成物は、後塩素化塩化ビニル系
樹脂が本来有する、耐熱性、耐薬品性、耐候性、耐燃性
とともに耐衝撃性及び加工性が優れたものであって、例
えば高温薬液用の容器やタンク、配管、あるいは温廃水
用下水配管、電カケープル保護管などの材料として特に
好適であシ、さらに、メッキ槽、塩素ガス配管、反応槽
などの窓板や、窓枠、壁板、パイプなどの建築・構築物
用部材などの用途にも有用である。Effects of the Invention The thermoplastic resin composition of the present invention has excellent heat resistance, chemical resistance, weather resistance, flame resistance, as well as impact resistance and processability, which are inherent to post-chlorinated vinyl chloride resins. For example, it is particularly suitable as a material for containers, tanks, piping for high-temperature chemical solutions, sewage piping for heated waste water, electrical cable protection pipes, etc. Furthermore, it is also suitable for use as window plates for plating tanks, chlorine gas piping, reaction tanks, etc. It is also useful for applications such as window frames, wall boards, pipes, and other building and construction components.
実施例
次に実施例により本発明をさらに詳細に°説明するが、
本発明はこれらの例によってなんら限定されるものでは
ない。EXAMPLES Next, the present invention will be explained in more detail with reference to Examples.
The present invention is not limited in any way by these examples.
なお、組成物の各物性は次の方法に従って評価した。In addition, each physical property of the composition was evaluated according to the following method.
試験片の作製
粉状コンパウンドを、8インチ−ロールミキサーを用い
て180t;、7分間混練し、約0.55藺のシートを
得、次いで、このシート2枚又は6枚を縦横の方向が交
互になるように重ね、190℃でプレス成形してそれぞ
れ厚さj txw又は3styの板状体を得たのち、こ
の板状体からそれぞれ試験片を切シ出した。Preparation of test pieces The powdered compound was kneaded for 7 minutes at 180 tons using an 8-inch roll mixer to obtain a sheet of approximately 0.55 mm. Next, 2 or 6 of these sheets were mixed in alternating vertical and horizontal directions. They were stacked so as to have the following shapes and press-molded at 190°C to obtain plate-shaped bodies each having a thickness of j txw or 3sty, and then test pieces were cut from each of the plate-shaped bodies.
(1)耐衝撃性
JIS K−7111に準拠して、シャルピー衝撃性試
験を行い、耐衝撃性を求めた。なお試験片は1 mm厚
の板状体より切り出した。(1) Impact resistance A Charpy impact test was conducted in accordance with JIS K-7111 to determine impact resistance. Note that the test piece was cut out from a plate with a thickness of 1 mm.
(2)耐熱性
JIS K−6745に準拠して、柔軟温度試験を行い
、耐熱性を求めた。なお、試験片は1間座の板状体より
切り出した。(2) Heat resistance A flexibility temperature test was conducted in accordance with JIS K-6745 to determine heat resistance. Note that the test piece was cut out from a plate-shaped body with one spacer.
(6)溶融粘度、持続熱安定性
粉状コンパウンド57gを、ブラベンダー社製プラスト
グラフ機の予め200℃に温調されたロータ一槽内に充
てんし、ニーダ−を5 Q rpmで回転させることに
より、該コンパウンドを溶融混練し、その安定状態にお
ける溶融抵抗値(トルク、kg−77+)を溶融粘度値
とし、また前記コンパウンドのゲル化開始から熱分解開
始までの時間(6)を持続熱安定性の値とした。(6) Fill 57 g of the powdered compound with melt viscosity and sustained heat stability into a rotor tank of a Brabender Plastograph machine whose temperature was pre-controlled at 200°C, and rotate the kneader at 5 Q rpm. The compound is melt-kneaded, the melt resistance value (torque, kg-77+) in the stable state is taken as the melt viscosity value, and the time (6) from the start of gelation of the compound to the start of thermal decomposition is the sustained thermal stability. The value was taken as the gender value.
(4) ロールシートゲル化性
予め180℃にセットされた8インチφ、20インチ長
のミキシングロール(2本)を15 rpm及びI B
rpmで回転させ、これに粉状コンノくランド150
!7を充てん、混練してシート状とし、その際のロール
加工性を観察して、次の判定基準に従いロールシートゲ
ル化性を評価した。(4) Roll sheet gelation properties Mixing rolls (2 rolls) with an 8-inch diameter and 20-inch length preset at 180°C at 15 rpm and IB
Rotate at rpm and add 150 powder powder to this
! 7 was filled and kneaded to form a sheet, the roll processability at that time was observed, and the roll sheet gelability was evaluated according to the following criteria.
(イ)粉状からシート状に巻き付くまでの時間。(a) Time from powder to rolled into sheet.
1分以内 二〇
1〜2分未満:■
2〜6分未満:△
6分以上 :×
(ロ) シート状に巻き付いてから、60分間混線後、
シートの剥離状態を観察。Within 1 minute 201 to less than 2 minutes: ■ 2 to less than 6 minutes: △ 6 minutes or more: × (B) After being wrapped in a sheet, after 60 minutes of crosstalk,
Observe the peeling state of the sheet.
剥離性が良好 二〇
” やや悪い:■
” 悪い :△
ロールに粘着 :×
(5)耐化学薬品性
60重量係クロム酸水溶液、80重量%硫酸水溶液及び
20重量係硝酸水溶液をそれぞれ調製して、液温を60
℃に保ち、それぞれの溶液中に試験片(25X80X3
問)を2週間浸せき後、流水で2時間洗浄し、デシケー
タ中で48時間保持したのち、その曲げ弾性率を訂S
K−7203に準拠して測定し、次の基準に従い、耐化
学薬品性を評価した。Good peelability 20" Slightly poor: ■ " Bad: △ Adhesive to roll: × (5) Chemical resistance A 60 weight percent chromic acid aqueous solution, an 80 weight percent sulfuric acid aqueous solution, and a 20 weight percent nitric acid aqueous solution were prepared. , set the liquid temperature to 60
℃, test pieces (25X80X3
Question) was soaked for 2 weeks, washed with running water for 2 hours, kept in a desiccator for 48 hours, and its flexural modulus was determined.
Measurement was conducted in accordance with K-7203, and chemical resistance was evaluated in accordance with the following criteria.
弾性率の変化が5q6未満 二 〇5〜10チ未満
: △
10%以上: ×
実施例1,2、比較例1,2
平均塩素含有量61o8重量係の後塩素化塩化ビニル系
樹脂(cpvc ) 1oo重量部、耐衝撃性改良剤と
してのMBS系樹脂〔フレ・・BTA lTlNx %
具現化学(株)製)0,4,8.12重量部、安定剤(
三塩基性硫酸鉛〕6重量部及び滑剤(ステアリン酸鉛)
1重量部を、らいかい機を用いて120℃で、15分間
混合したのち、取シ出し冷却して粉状コンパウンドを調
製し、このものについてl性を求めた。その結果を第1
表に示す。Change in elastic modulus is less than 5q6 205 to less than 10%: △ 10% or more: × Examples 1, 2, Comparative Examples 1, 2 Average chlorine content 61o8 weight ratio chlorinated vinyl chloride resin (CPVC) 100 parts by weight, MBS resin as impact modifier [Fure...BTA lTlNx %
Manufactured by Gugen Kagaku Co., Ltd.) 0, 4, 8.12 parts by weight, stabilizer (
Tribasic lead sulfate] 6 parts by weight and lubricant (lead stearate)
1 part by weight was mixed for 15 minutes at 120° C. using a sieve machine, taken out and cooled to prepare a powdery compound, and the lactic properties of this compound were determined. The result is the first
Shown in the table.
なお、比較例1はMBS系樹脂配合量が0の場合、実施
例1及び2はそれぞれ4及び8重量部の場合、比較例2
は12重量部の場合である。In addition, Comparative Example 1 is when the MBS resin content is 0, Examples 1 and 2 are 4 and 8 parts by weight, respectively, Comparative Example 2 is
is the case of 12 parts by weight.
比較例6
実施例2において、平均塩素含有量が61o8重量係の
cpvcの代りに、平均塩素含有量が66.6重量%の
cpvcとpvc (塩素含有量56゜8重量%)とを
重量比50150の割合でブレンドしたもの(平均塩素
含有量61゜6重量%)を用いた以外は、実施例2と同
様にして粉状コンパウンドを調製し、その物註を求めた
。結果を第1表に示す。Comparative Example 6 In Example 2, instead of CPVC with an average chlorine content of 61°8 weight ratio, CPVC with an average chlorine content of 66.6% by weight and PVC (chlorine content 56°8% by weight) were used in the weight ratio. A powdered compound was prepared in the same manner as in Example 2, except that a blend of 50,150% (average chlorine content: 61.6% by weight) was used, and its characteristics were determined. The results are shown in Table 1.
実施例6,4、比較例4,5
平均塩素含有量61゜8重量%のcpvcの代シに、平
均塩素含有量66゜6重量%のCPVCを用いた以外は
、それぞれ実施例1,2、比較例1,2と同様にして粉
状コンパウンドを調製し、それらの物性を求めた。結果
を第1表に示す。Examples 6 and 4, Comparative Examples 4 and 5 Examples 1 and 2, respectively, except that CPVC with an average chlorine content of 66.6% by weight was used instead of CPVC with an average chlorine content of 61.8% by weight. Powdered compounds were prepared in the same manner as in Comparative Examples 1 and 2, and their physical properties were determined. The results are shown in Table 1.
比較例6
比較例乙において、平均塩素含有量る6゜3重量係ノC
PVCとPvCとのブレンド比を、重量基準で70/6
0(ブレンド物の平均塩素含有量63.5重量%)と変
えた以外は、比較例6と同様にして粉状コンパウンドを
調製し、その物性を求めた。結果を第1表に示す。Comparative Example 6 In Comparative Example B, the average chlorine content is 6°3 weight ratio C
The blend ratio of PVC and PvC is 70/6 on a weight basis.
A powdery compound was prepared in the same manner as in Comparative Example 6, except that the average chlorine content of the blend was changed to 0 (average chlorine content of the blend: 63.5% by weight), and its physical properties were determined. The results are shown in Table 1.
実施例5〜8、比較例7〜10
耐衝撃性改良剤としてMBS系樹脂を用いる代りに、多
成分アクリルゴム系樹脂〔フレ・・旧A−28、具現化
学(絹製〕を用いた以外は、それぞれ実施例1〜4、比
較例2,3.5.6と同様にして粉状コンパウンドを調
製し、それらの物性を求めた。その結果を第2表に示す
。Examples 5 to 8, Comparative Examples 7 to 10 Instead of using MBS resin as an impact modifier, multi-component acrylic rubber resin [Fure...formerly A-28, Guji Kagaku (made from silk)] was used. Powdered compounds were prepared in the same manner as in Examples 1 to 4 and Comparative Examples 2, 3, 5, and 6, respectively, and their physical properties were determined.The results are shown in Table 2.
実施例9〜12、比較例11〜14
耐衝撃性改良剤として、MBS系樹脂を用いる代りに、
後塩素化ポリエチレン〔エラスレン651へ昭和電工(
株)製〕を用いた以外は、それぞれ実施例1〜4、比較
例2.3.5.6と同様にして、粉状コンパウンドを調
製し、それらの物性を求めた。その結果を第3表に示す
。Examples 9 to 12, Comparative Examples 11 to 14 Instead of using MBS resin as an impact modifier,
Post-chlorinated polyethylene [Showa Denko to Elaslene 651 (
Powdered compounds were prepared in the same manner as in Examples 1 to 4 and Comparative Example 2.3.5.6, respectively, except that the compound manufactured by Co., Ltd. was used, and their physical properties were determined. The results are shown in Table 3.
実施例16〜16、比較例15〜18
耐衝撃改良剤として、MBS系樹脂を用いる代りに、E
VA系樹脂〔エバフレックス11250、三井ポリケミ
カル(株)製〕を用いた以外は、それぞれ実施例1〜4
.比較例2,3,5.6と同様にして粉状コンパウンド
を調製し、それらの物性を求めた。その結果を第4表に
示す。Examples 16-16, Comparative Examples 15-18 Instead of using MBS resin as an impact modifier, E
Examples 1 to 4, respectively, except that VA-based resin [Evaflex 11250, manufactured by Mitsui Polychemical Co., Ltd.] was used.
.. Powdered compounds were prepared in the same manner as in Comparative Examples 2, 3, and 5.6, and their physical properties were determined. The results are shown in Table 4.
手続補正帯
昭和62年5月7日
特許庁長官 黒 1)明 雄 殿
1、事件の表示
昭和62年特許願第83003号
2、発明の名称
耐熱性熱可塑性樹脂組成物
3、補正をする者
事件との関係 特許出願人
東京都千代田区丸の内三丁目3番1号
日本カーバイド工業株式会社
代表者 神 谷 正 −
4、代理人
電話(591)991.0番1;’、V1弓」−斗5、
補正命令の日付 自 発
6、補正により増加する発明の数 0
8、補正の内容
(1)明細書第8ページ第5行及び第9ペーノ第2〜3
行の1三菱レーヨン」を「三菱レイヨン」に訂正します
。Procedural amendment band May 7, 1988 Commissioner of the Patent Office Black 1) Akio Yu 1, Indication of the case Patent Application No. 83003 of 1983 2, Name of the invention Heat-resistant thermoplastic resin composition 3, Person making the amendment Relationship to the incident Patent applicant: 3-3-1 Marunouchi, Chiyoda-ku, Tokyo Representative: Tadashi Kamiya - 4, agent telephone: (591) 991.0-1;', V1 Yumi' - To 5,
Date of amendment order: 6, Number of inventions increased by amendment: 0 8, Contents of amendment (1) Specification, page 8, line 5, and page 9, lines 2 to 3
Correct line 1 "Mitsubishi Rayon" to "Mitsubishi Rayon."
(2)同第9ペーノ第4行の1カネ力エースB−56」
を1カネエースB−564に訂正します。(2) 1 money power ace B-56 in the 4th row of the 9th peno
Correct it to 1 Money Ace B-564.
(3) 同第10ペーノ第15行の「クリスタルワラカ
ス、ポリエチレンワラカス」を1クリスタルワツクス、
ポリエチレンワックス」に訂正します。(3) 1 crystal wax of "crystal wax, polyethylene wax" in line 15 of the 10th peno.
Corrected to "Polyethylene wax."
(4) 同第13ページ第7行の1ライカイキ」を「ら
いかい磯。1に訂正します。(4) In the 7th line of page 13, 1 Laikaiki” is corrected to 1.
(5)同第14ページ下から2行目の1試験片は1yu
Jを1試験片は3〃m」に訂正します。(5) 1 test piece on the second line from the bottom of page 14 is 1yu
Correct J to 1 test piece is 3 m.
(6)同第21ページ第2表の比較例10の欄、物性評
価の持続熱安定性の項(、oi、、)r△」を「10」
に、評価「10」を「△」にそれぞれ訂正します。(6) In the Comparative Example 10 column of Table 2 on page 21, the sustained thermal stability term (,oi,,)r△” in the physical property evaluation is set to “10”.
We will correct the rating from ``10'' to ``△''.
Claims (1)
満の後塩素化塩化ビニル系樹脂100重量部に対して、
(B)耐衝撃性改良剤2〜10重量部を配合して成る、
良好な加工性をもつ耐熱性熱可塑性樹脂組成物。 2 後塩素化塩化ビニル系樹脂が、JISK−6721
に従って測定したニトロベンゼン法による固有粘度0。 27〜0。 44を有するものである特許請求の範囲第1項記載の組
成物。 6 耐衝撃性改良剤が多成分アクリルゴム系樹脂、後塩
素化ポリエチレン、メチルメタクリレート・ブタジエン
・スチレン系樹脂及びエチレン・酢酸ビニル系樹脂の中
から選ばれた少なくとも1種である特許請求の範囲第1
項又は第2項記載の組成物。 4 熱溶融粘度が3kg・m以下である特許請求の範囲
第1項、第2項又は第3項記載の組成物。[Scope of Claims] 1(A) Based on 100 parts by weight of post-chlorinated vinyl chloride resin having an average chlorine content of 60% by weight or more and less than 64% by weight,
(B) containing 2 to 10 parts by weight of an impact modifier;
A heat-resistant thermoplastic resin composition with good processability. 2 The post-chlorinated vinyl chloride resin conforms to JISK-6721
Intrinsic viscosity 0 according to the nitrobenzene method measured according to the method. 27-0. 44. The composition according to claim 1, which has a molecular weight of 44. 6. Claim No. 6, wherein the impact modifier is at least one selected from a multicomponent acrylic rubber resin, a post-chlorinated polyethylene, a methyl methacrylate-butadiene-styrene resin, and an ethylene-vinyl acetate resin. 1
The composition according to item 1 or 2. 4. The composition according to claim 1, 2 or 3, which has a hot melt viscosity of 3 kg·m or less.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62083003A JP2521284B2 (en) | 1987-04-06 | 1987-04-06 | Heat resistant thermoplastic resin composition |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62083003A JP2521284B2 (en) | 1987-04-06 | 1987-04-06 | Heat resistant thermoplastic resin composition |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS63251449A true JPS63251449A (en) | 1988-10-18 |
JP2521284B2 JP2521284B2 (en) | 1996-08-07 |
Family
ID=13790081
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP62083003A Expired - Fee Related JP2521284B2 (en) | 1987-04-06 | 1987-04-06 | Heat resistant thermoplastic resin composition |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2521284B2 (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02142845A (en) * | 1988-11-24 | 1990-05-31 | Sekisui Chem Co Ltd | Chlorinated vinyl chloride resin composition |
JPH03152147A (en) * | 1989-11-07 | 1991-06-28 | Sekisui Chem Co Ltd | Rigid chlorinated vinyl chloride-based resin composition for injection molding |
WO1998054002A1 (en) * | 1997-05-27 | 1998-12-03 | Mitsubishi Plastics Inc. | Non-contact ic card and method for manufacturing the same |
WO2002064675A1 (en) * | 2001-02-16 | 2002-08-22 | Kaneka Corporation | Chlorinated vinyl chloride resin composition |
CN103351560A (en) * | 2013-07-11 | 2013-10-16 | 安徽玉发塑业有限公司 | CPVC (Chlorinated Polyvinyl Chloride) pipe |
JP2018509519A (en) * | 2015-03-24 | 2018-04-05 | サビック グローバル テクノロジーズ ベスローテン フェンノートシャップ | Polysiloxane-polycarbonate copolymer composition |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4842205A (en) * | 1971-10-01 | 1973-06-20 | ||
JPS4918102A (en) * | 1972-04-17 | 1974-02-18 | ||
JPS52972A (en) * | 1975-06-24 | 1977-01-06 | Asahi Dow Ltd | Dyeing of olefin foams |
JPS54141837A (en) * | 1978-04-26 | 1979-11-05 | Sekisui Chem Co Ltd | Chlorinated vinyl chloride resin composition |
-
1987
- 1987-04-06 JP JP62083003A patent/JP2521284B2/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4842205A (en) * | 1971-10-01 | 1973-06-20 | ||
JPS4918102A (en) * | 1972-04-17 | 1974-02-18 | ||
JPS52972A (en) * | 1975-06-24 | 1977-01-06 | Asahi Dow Ltd | Dyeing of olefin foams |
JPS54141837A (en) * | 1978-04-26 | 1979-11-05 | Sekisui Chem Co Ltd | Chlorinated vinyl chloride resin composition |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02142845A (en) * | 1988-11-24 | 1990-05-31 | Sekisui Chem Co Ltd | Chlorinated vinyl chloride resin composition |
JPH03152147A (en) * | 1989-11-07 | 1991-06-28 | Sekisui Chem Co Ltd | Rigid chlorinated vinyl chloride-based resin composition for injection molding |
WO1998054002A1 (en) * | 1997-05-27 | 1998-12-03 | Mitsubishi Plastics Inc. | Non-contact ic card and method for manufacturing the same |
WO2002064675A1 (en) * | 2001-02-16 | 2002-08-22 | Kaneka Corporation | Chlorinated vinyl chloride resin composition |
CN103351560A (en) * | 2013-07-11 | 2013-10-16 | 安徽玉发塑业有限公司 | CPVC (Chlorinated Polyvinyl Chloride) pipe |
JP2018509519A (en) * | 2015-03-24 | 2018-04-05 | サビック グローバル テクノロジーズ ベスローテン フェンノートシャップ | Polysiloxane-polycarbonate copolymer composition |
Also Published As
Publication number | Publication date |
---|---|
JP2521284B2 (en) | 1996-08-07 |
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