WO2017170985A1 - 積層チューブ - Google Patents
積層チューブ Download PDFInfo
- Publication number
- WO2017170985A1 WO2017170985A1 PCT/JP2017/013541 JP2017013541W WO2017170985A1 WO 2017170985 A1 WO2017170985 A1 WO 2017170985A1 JP 2017013541 W JP2017013541 W JP 2017013541W WO 2017170985 A1 WO2017170985 A1 WO 2017170985A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polyamide
- acid
- value
- copolymer
- mass
- Prior art date
Links
- 229920002647 polyamide Polymers 0.000 claims abstract description 479
- 239000004952 Polyamide Substances 0.000 claims abstract description 477
- 229920006012 semi-aromatic polyamide Polymers 0.000 claims abstract description 308
- 239000000203 mixture Substances 0.000 claims abstract description 240
- 229920000642 polymer Polymers 0.000 claims abstract description 191
- 239000004953 Aliphatic polyamide Substances 0.000 claims abstract description 57
- 229920003231 aliphatic polyamide Polymers 0.000 claims abstract description 57
- 125000003368 amide group Chemical group 0.000 claims abstract description 43
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 43
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 claims abstract description 42
- 150000001875 compounds Chemical class 0.000 claims abstract description 31
- 125000004018 acid anhydride group Chemical group 0.000 claims abstract description 19
- -1 polyhexamethylene Polymers 0.000 claims description 486
- 229920001577 copolymer Polymers 0.000 claims description 244
- 229910052731 fluorine Inorganic materials 0.000 claims description 134
- 239000000178 monomer Substances 0.000 claims description 130
- 239000011737 fluorine Substances 0.000 claims description 122
- 229920000299 Nylon 12 Polymers 0.000 claims description 121
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 117
- ILRSCQWREDREME-UHFFFAOYSA-N dodecanamide Chemical compound CCCCCCCCCCCC(N)=O ILRSCQWREDREME-UHFFFAOYSA-N 0.000 claims description 85
- 229920000572 Nylon 6/12 Polymers 0.000 claims description 80
- 125000000524 functional group Chemical group 0.000 claims description 76
- 229920002292 Nylon 6 Polymers 0.000 claims description 58
- 125000004432 carbon atom Chemical group C* 0.000 claims description 55
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 48
- 229920006111 poly(hexamethylene terephthalamide) Polymers 0.000 claims description 40
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 36
- GVNWZKBFMFUVNX-UHFFFAOYSA-N Adipamide Chemical compound NC(=O)CCCCC(N)=O GVNWZKBFMFUVNX-UHFFFAOYSA-N 0.000 claims description 35
- KKEYFWRCBNTPAC-UHFFFAOYSA-N terephthalic acid group Chemical group C(C1=CC=C(C(=O)O)C=C1)(=O)O KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 33
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 32
- 125000003277 amino group Chemical group 0.000 claims description 32
- 239000002994 raw material Substances 0.000 claims description 31
- 150000001408 amides Chemical class 0.000 claims description 29
- 125000001142 dicarboxylic acid group Chemical group 0.000 claims description 26
- 229920006152 PA1010 Polymers 0.000 claims description 25
- 125000004427 diamine group Chemical group 0.000 claims description 25
- 230000009257 reactivity Effects 0.000 claims description 24
- 239000000446 fuel Substances 0.000 claims description 22
- FJXWKBZRTWEWBJ-UHFFFAOYSA-N nonanediamide Chemical compound NC(=O)CCCCCCCC(N)=O FJXWKBZRTWEWBJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000011231 conductive filler Substances 0.000 claims description 21
- 229920006121 Polyxylylene adipamide Polymers 0.000 claims description 14
- 229920005992 thermoplastic resin Polymers 0.000 claims description 14
- 229920000571 Nylon 11 Polymers 0.000 claims description 12
- 229920001519 homopolymer Polymers 0.000 claims description 12
- GKXVJHDEWHKBFH-UHFFFAOYSA-N xylylenediamine group Chemical group C=1(C(=CC=CC1)CN)CN GKXVJHDEWHKBFH-UHFFFAOYSA-N 0.000 claims description 12
- WPWNSTTVSOUHRP-UHFFFAOYSA-N [1-(aminomethyl)naphthalen-2-yl]methanamine Chemical group C1=CC=CC2=C(CN)C(CN)=CC=C21 WPWNSTTVSOUHRP-UHFFFAOYSA-N 0.000 claims description 11
- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 claims description 11
- 229920006396 polyamide 1012 Polymers 0.000 claims description 10
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical group C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 claims description 9
- 229920006123 polyhexamethylene isophthalamide Polymers 0.000 claims description 6
- 239000011342 resin composition Substances 0.000 claims description 2
- 150000003346 selenoethers Chemical class 0.000 claims 1
- 229920001971 elastomer Polymers 0.000 abstract description 43
- 239000000806 elastomer Substances 0.000 abstract description 42
- 239000000470 constituent Substances 0.000 abstract description 17
- 239000010410 layer Substances 0.000 description 129
- 238000004519 manufacturing process Methods 0.000 description 127
- 238000006116 polymerization reaction Methods 0.000 description 107
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 87
- 125000006367 bivalent amino carbonyl group Chemical group [H]N([*:1])C([*:2])=O 0.000 description 81
- 238000000034 method Methods 0.000 description 72
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 description 61
- 239000000126 substance Substances 0.000 description 59
- ALBYIUDWACNRRB-UHFFFAOYSA-N hexanamide Chemical compound CCCCCC(N)=O ALBYIUDWACNRRB-UHFFFAOYSA-N 0.000 description 49
- 229920005989 resin Polymers 0.000 description 44
- 239000011347 resin Substances 0.000 description 44
- 229910052698 phosphorus Inorganic materials 0.000 description 42
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 40
- 239000008188 pellet Substances 0.000 description 40
- 238000006243 chemical reaction Methods 0.000 description 39
- 238000002844 melting Methods 0.000 description 38
- 230000008018 melting Effects 0.000 description 38
- 238000012545 processing Methods 0.000 description 36
- 238000002360 preparation method Methods 0.000 description 35
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 34
- 239000005977 Ethylene Substances 0.000 description 34
- 239000003963 antioxidant agent Substances 0.000 description 34
- 230000003078 antioxidant effect Effects 0.000 description 34
- 230000004888 barrier function Effects 0.000 description 34
- 239000000243 solution Substances 0.000 description 34
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 33
- 239000011574 phosphorus Substances 0.000 description 33
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 32
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 32
- 239000003381 stabilizer Substances 0.000 description 32
- 239000011229 interlayer Substances 0.000 description 31
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 22
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 19
- 239000004760 aramid Substances 0.000 description 19
- 229920003235 aromatic polyamide Polymers 0.000 description 19
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 18
- MXAOILAHPVJWBS-UHFFFAOYSA-N 10-(azepan-1-yl)-10-oxodecanamide Chemical compound NC(=O)CCCCCCCCC(=O)N1CCCCCC1 MXAOILAHPVJWBS-UHFFFAOYSA-N 0.000 description 17
- 239000002253 acid Substances 0.000 description 17
- 239000003502 gasoline Substances 0.000 description 17
- 229920002554 vinyl polymer Polymers 0.000 description 17
- 125000005587 carbonate group Chemical group 0.000 description 16
- 230000002829 reductive effect Effects 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 229910052783 alkali metal Inorganic materials 0.000 description 15
- 150000001412 amines Chemical class 0.000 description 15
- PGGROMGHWHXWJL-UHFFFAOYSA-N 4-(azepane-1-carbonyl)benzamide Chemical compound C1=CC(C(=O)N)=CC=C1C(=O)N1CCCCCC1 PGGROMGHWHXWJL-UHFFFAOYSA-N 0.000 description 14
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 14
- 150000004985 diamines Chemical class 0.000 description 14
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 14
- 238000000465 moulding Methods 0.000 description 14
- 125000004430 oxygen atom Chemical group O* 0.000 description 14
- 150000003839 salts Chemical class 0.000 description 14
- 125000001153 fluoro group Chemical group F* 0.000 description 13
- 238000004898 kneading Methods 0.000 description 13
- 239000007788 liquid Substances 0.000 description 13
- 239000003505 polymerization initiator Substances 0.000 description 13
- 239000007790 solid phase Substances 0.000 description 13
- 238000003756 stirring Methods 0.000 description 13
- OFNISBHGPNMTMS-UHFFFAOYSA-N 3-methylideneoxolane-2,5-dione Chemical compound C=C1CC(=O)OC1=O OFNISBHGPNMTMS-UHFFFAOYSA-N 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 12
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 12
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 description 12
- 239000012530 fluid Substances 0.000 description 12
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical group NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 description 12
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 12
- GVNVAWHJIKLAGL-UHFFFAOYSA-N 2-(cyclohexen-1-yl)cyclohexan-1-one Chemical compound O=C1CCCCC1C1=CCCCC1 GVNVAWHJIKLAGL-UHFFFAOYSA-N 0.000 description 11
- GAGWMWLBYJPFDD-UHFFFAOYSA-N 2-methyloctane-1,8-diamine Chemical group NCC(C)CCCCCCN GAGWMWLBYJPFDD-UHFFFAOYSA-N 0.000 description 11
- FQLAJSQGBDYBAL-UHFFFAOYSA-N 3-(azepane-1-carbonyl)benzamide Chemical compound NC(=O)C1=CC=CC(C(=O)N2CCCCCC2)=C1 FQLAJSQGBDYBAL-UHFFFAOYSA-N 0.000 description 11
- 101150065749 Churc1 gene Proteins 0.000 description 11
- ZDXPYRJPNDTMRX-GSVOUGTGSA-N D-glutamine Chemical compound OC(=O)[C@H](N)CCC(N)=O ZDXPYRJPNDTMRX-GSVOUGTGSA-N 0.000 description 11
- 102100038239 Protein Churchill Human genes 0.000 description 11
- 125000001931 aliphatic group Chemical group 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 11
- NFVUAUVSFDFOJT-UHFFFAOYSA-N octanediamide Chemical compound NC(=O)CCCCCCC(N)=O NFVUAUVSFDFOJT-UHFFFAOYSA-N 0.000 description 11
- 229920006128 poly(nonamethylene terephthalamide) Polymers 0.000 description 11
- 230000000379 polymerizing effect Effects 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- DJZKNOVUNYPPEE-UHFFFAOYSA-N tetradecane-1,4,11,14-tetracarboxamide Chemical compound NC(=O)CCCC(C(N)=O)CCCCCCC(C(N)=O)CCCC(N)=O DJZKNOVUNYPPEE-UHFFFAOYSA-N 0.000 description 11
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 10
- 229920001400 block copolymer Polymers 0.000 description 10
- 239000006229 carbon black Substances 0.000 description 10
- 235000019241 carbon black Nutrition 0.000 description 10
- 238000010828 elution Methods 0.000 description 10
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 10
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 10
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 9
- 239000002033 PVDF binder Substances 0.000 description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 9
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 9
- 125000004437 phosphorous atom Chemical group 0.000 description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 9
- KHXKESCWFMPTFT-UHFFFAOYSA-N 1,1,1,2,2,3,3-heptafluoro-3-(1,2,2-trifluoroethenoxy)propane Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)F KHXKESCWFMPTFT-UHFFFAOYSA-N 0.000 description 8
- PBLZLIFKVPJDCO-UHFFFAOYSA-N 12-aminododecanoic acid Chemical compound NCCCCCCCCCCCC(O)=O PBLZLIFKVPJDCO-UHFFFAOYSA-N 0.000 description 8
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- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 8
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 description 8
- 150000001735 carboxylic acids Chemical class 0.000 description 8
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 8
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 8
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 8
- 239000003921 oil Substances 0.000 description 8
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 8
- 229920000768 polyamine Polymers 0.000 description 8
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 8
- 229920003048 styrene butadiene rubber Polymers 0.000 description 8
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 8
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 7
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 7
- 229920000459 Nitrile rubber Polymers 0.000 description 7
- 150000001340 alkali metals Chemical class 0.000 description 7
- 125000004202 aminomethyl group Chemical group [H]N([H])C([H])([H])* 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 125000003700 epoxy group Chemical group 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000000704 physical effect Effects 0.000 description 7
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 description 6
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 6
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000004609 Impact Modifier Substances 0.000 description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 229920003189 Nylon 4,6 Polymers 0.000 description 6
- 239000004734 Polyphenylene sulfide Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
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- 239000001361 adipic acid Substances 0.000 description 6
- 235000011037 adipic acid Nutrition 0.000 description 6
- 125000002723 alicyclic group Chemical group 0.000 description 6
- 150000001339 alkali metal compounds Chemical class 0.000 description 6
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 6
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 6
- ZWUNKULTLYLLTH-UHFFFAOYSA-N cyclohexane-1,4-dicarboxamide Chemical compound NC(=O)C1CCC(C(N)=O)CC1 ZWUNKULTLYLLTH-UHFFFAOYSA-N 0.000 description 6
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 6
- 230000006866 deterioration Effects 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
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- 238000010528 free radical solution polymerization reaction Methods 0.000 description 6
- 125000005067 haloformyl group Chemical group 0.000 description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 6
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 6
- QZUPTXGVPYNUIT-UHFFFAOYSA-N isophthalamide Chemical compound NC(=O)C1=CC=CC(C(N)=O)=C1 QZUPTXGVPYNUIT-UHFFFAOYSA-N 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- BNJOQKFENDDGSC-UHFFFAOYSA-N octadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCC(O)=O BNJOQKFENDDGSC-UHFFFAOYSA-N 0.000 description 6
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 6
- 229920002492 poly(sulfone) Polymers 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 229920001470 polyketone Polymers 0.000 description 6
- 229920005672 polyolefin resin Polymers 0.000 description 6
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino-carboxylic acids or of polyamines and polycarboxylic acids
Definitions
- the present invention relates to a laminated tube.
- the main material is metal, excellent corrosion resistance, and lightweight resin in response to problems of rusting due to road antifreeze agents, global warming prevention, and energy saving since old times Alternatives to are in progress.
- a resin used as a tube for piping polyamide resin, saturated polyester resin, polyolefin resin, thermoplastic polyurethane resin etc. may be mentioned.
- heat resistance and resistance The applicable range was limited because the drug property and the like were insufficient.
- tubes for automobile piping use oxygen-containing gasoline blended with low boiling point alcohols such as methanol and ethanol or ethers such as ethyl-t-butyl ether (ETBE) from the viewpoint of saving consumption of gasoline and improving performance. Etc. are transported.
- ETBE ethyl-t-butyl ether
- strict exhaust gas regulations including the prevention of leakage to the atmosphere due to the diffusion of volatile hydrocarbons and the like through the pipe tube partition have been implemented.
- a single-layer tube using polyamide-based resin conventionally used, in particular, polyamide 11 or polyamide 12 excellent in strength, toughness, chemical resistance, flexibility, etc. alone is the above-mentioned
- the barrier property to the chemical solution is not sufficient, and in particular, improvement to the alcohol-containing gasoline barrier property is required.
- resins having good chemical liquid barrier properties such as saponified ethylene / vinyl acetate copolymer (EVOH), polymetaxylylene adipamide (polyamide MXD6), polybutylene terephthalate (PBT), polyethylene Naphthalate (PEN), polybutylene naphthalate (PBN), polyphenylene sulfide (PPS), polyvinylidene fluoride (PVDF), ethylene / tetrafluoroethylene copolymer (ETFE), ethylene / chlorotrifluoroethylene copolymer (ECTFE) ), Tetrafluoroethylene / hexafluoropropylene copolymer (TFE / HFP, FEP), tetrafluoroethylene / hexafluoropropylene / vinylidene fluoride copolymer (TFE / HFP / VDF, THV), tetrahydrofuran (Ethylene
- molded articles using polyamide resin, particularly nylon 11 or nylon 12 excellent in strength, toughness, chemical resistance and flexibility, as the innermost layer, which are conventionally used, are monomers or the like by contact with the fuel. It has been confirmed that low molecular weight components such as oligomers gradually dissolve and precipitate in the fuel, and the engine start can not be generated due to the adhesion to the moving parts of the injector and fuel tank valve, and the internal pressure control of the fuel tank Potential problems are pointed out.
- Polynonamethylene terephthalamide (PA9T) attracts attention as a low specific gravity, low cost tube component excellent in chemical liquid barrier properties and elution resistance of monomers and oligomers.
- the present inventors have found that a layer comprising aliphatic polyamide, a diamine unit containing 60 mol% or more of 1,9-nonanediamine unit and / or 2-methyl-1,8-octanediamine unit with respect to all diamine units,
- a laminate comprising at least two layers comprising a semiaromatic polyamide layer comprising a dicarboxylic acid unit containing 60% by mole or more of terephthalic acid unit and / or naphthalenedicarboxylic acid unit based on all dicarboxylic acid units
- Patent Documents 2 to 5 A structure is proposed (see Patent Documents 2 to 5).
- a layer made of an aliphatic polyamide such as polyamide 12 polynonamethylene terephthalamide having excellent chemical solution barrier properties
- a laminated tube has been proposed which has a layer composed of a semiaromatic polyamide composition containing a specific organic acid salt (organic acid salt having 10 to 24 carbon atoms) in a semiaromatic polyamide such as amide (PA9T) (See Patent Document 6).
- the object of the present invention is to solve the above problems and maintain chemical resistance, interlayer adhesion, and durability while maintaining various properties such as chemical liquid barrier property, low temperature impact resistance, elution resistance of monomer and oligomer.
- An object of the present invention is to provide an excellent laminated tube.
- the present inventors include a semiaromatic polyamide composition containing a layer containing a specific aliphatic polyamide composition and a semiaromatic polyamide having a specific structure.
- the present invention A two or more layered tube comprising (a) a layer and (b) a layer, wherein At least one set of said (a) layer and said (b) layer being arranged adjacent to each other,
- the (a) layer contains an aliphatic polyamide composition (A)
- the (b) layer contains a semiaromatic polyamide composition (B)
- the aliphatic polyamide composition (A) comprises a polyamide (A1), a polyamide (A2), and an elastomeric polymer (A3)
- the polyamide (A1) is an aliphatic polyamide having a ratio of the number of methylene groups to the number of amide groups of 8.0 or more, and is contained in the aliphatic polyamide composition (A) in an amount of 40% by mass to 90% by mass.
- the polyamide (A2) is a polyamide other than the polyamide (A1), and is contained in the aliphatic polyamide composition (A) in an amount of 5% by mass to 30% by mass.
- the elastomeric polymer (A3) contains a structural unit derived from an unsaturated compound having a carboxyl group and / or an acid anhydride group, and it is contained in an amount of 5 to 30% by mass in the aliphatic polyamide composition (A).
- the semiaromatic polyamide composition (B) comprises a semiaromatic polyamide (B1) or a semiaromatic polyamide (B2), 60% by mass or more of the semiaromatic polyamide (B1) or the semiaromatic polyamide (B2) is contained in the semiaromatic polyamide composition (B),
- the semiaromatic polyamide (B1) contains 50 mol% or more of an aliphatic diamine unit having 9 or 10 carbon atoms with respect to all diamine units of the semiaromatic polyamide (B1), 50% by mole or more of terephthalic acid units and / or naphthalenedicarboxylic acid units with respect to all the dicarboxylic acid units of B1),
- the polyamide (A1) is polyhexamethylene dodecamide (polyamide 612), polynonamethylene dodecamide (polyamide 912), polydecamethylene sebacamide (polyamide 1010), polydecamethylene dodecamide (polyamide 1012) And / or at least one homopolymer selected from the group consisting of polydodecamethylene dodecamide (polyamide 1212), polyundecanamide (polyamide 11), and polydodecane amide (polyamide 12), and / or raw material singles forming these.
- a laminated tube which is a copolymer using several kinds of monomers.
- the polyamide (A2) is polycaproamide (polyamide 6), polyhexamethylene adipamide (polyamide 66), polyhexamethylene azelamide (polyamide 69), polyhexamethylene sebacamide (polyamide 610), At least one homopolymer selected from the group consisting of polyhexamethylene terephthalamide (polyamide 6T), polyhexamethylene isophthalamide (polyamide 6I), and polymethaxylylene adipamide (polyamide MXD6), and / or Copolymers using several kinds of raw material monomers for forming these, or polycaproamide (polyamide 6), polyhexamethylene adipamide (polyamide 66), polyhexamethylene aceramide (polyamide 69), poly Hexamethylene sebacamide (polyamide 6) 0) A raw material single material forming at least one selected from the group consisting of polyhexamethylene terephthalamide (polyamide 6T), polyhexamethylene
- the terminal amino group concentration per gram of each of the polyamide (A1) and the polyamide (A2) in the aliphatic polyamide composition (A) is [A] ( ⁇ eq / g), and the terminal carboxyl group concentration is B] ([mu] eq / g), [A]> [B] + 10, a laminated tube.
- the (c) layer is a laminated tube containing a fluorine-containing polymer (C) in which a functional group having reactivity to an amino group is introduced into a molecular chain.
- C fluorine-containing polymer
- a laminated tube in which the innermost layer is a conductive layer containing a thermoplastic resin composition containing a conductive filler.
- Aliphatic polyamide composition (A) contains polyamide (A1), polyamide (A2), and elastomer polymer (A3), and polyamide (A1) is a fat having a ratio of the number of methylene groups to the number of amide groups of 8.0 or more Aliphatic polyamide composition (A), which is contained in an amount of 40% by mass to 90% by mass, and the polyamide (A2) is a polyamide other than the above-mentioned polyamide (A1); A) contains 5% by mass or more and 30% by mass or less, and the elastomer polymer (A3) contains a constituent unit derived from an unsaturated compound having a carboxyl group and / or an acid anhydride group, and is aliphatic The polyamide composition (A) contains 5% by mass to 30% by mass, and the solubility parameter SP of the polyamide (A1) and the polyamide (A2) is contained.
- ] is 1/2 1.8 to 5.5 (MPa) (hereinafter, aliphatic It may be called polyamide composition (A).
- the aliphatic polyamide composition (A) does not contain a plasticizer from the viewpoint of durability of interlayer adhesion after contact and immersion in fuel for a long time and / or after heat treatment.
- the polyamide (A1) contains only an aliphatic group in the repeating unit and has an amide bond (-CONH-) in the main chain, and the ratio of the number of methylene groups ([CH 2 ]) to the number of amide groups ([NHCO]) [CH 2 ] / [NHCO] (hereinafter, the ratio of the number of methylene groups to the number of amide groups may be referred to as [CH 2 ] / [NHCO]) is 8.0 or more (hereinafter referred to as polyamide (A1) There is a case.).
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups of the poly (dodecaneamide / dodecamethylene dodecamide) copolymer (polyamide 12/1212) is polydodecaneamide (polyamide 12) and polydodecamethylene Since the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups of dodecamide (polyamide 1212) is 11.0, regardless of the mass ratio of constituent repeating units and the molar ratio, the number of methylene groups is relative to the number of amide groups. The ratio [CH 2 ] / [NHCO] is 11.0.
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups of the poly (dodecaneamide / hexamethylene dodecamide) copolymer (polyamide 12/612) to the number of amide groups changes depending on the molar ratio of the constituent repeating units.
- the ratio of the number of methylene groups to the number of amide groups of polydodecane amide (polyamide 12) [CH 2 ] / [NHCO] is 11.0, and the ratio of the number of methylene groups to the number of amide groups of polyhexamethylene dodecamide (polyamide 612) [CH 2 ] / [NHCO] is 8.0, so that it can be calculated if the molar ratio of the repeating unit of the constituent unit is known, and the dodecane amide unit / hexamethylene dodecamide unit is 80:20 (mass ratio), 86.
- the ratio of the number of methylene groups to the number of amide groups decreases [CH 2 ] / [NHCO], but at least the ratio of the number of methylene groups to the number of amide groups [CH 2 ] / [NHCO] It never falls below 8.0.
- the number of amide groups of the number of methylene groups is The copolymer using several kinds of raw material monomers (constituting repeating units) forming an aliphatic polyamide having a ratio [CH 2 ] / [NHCO] of 8.0 or more does not depend on the molar ratio of the constituting repeating units.
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups is 8.0 or more, and is included in the polyamide (A1) of the present application.
- the polyamide (A1) has, as one component, a raw material monomer (constituting repeating unit) that forms an aliphatic polyamide having a ratio [CH 2 ] / [NHCO] of methylene groups to the number of amide groups of 8.0 or more.
- polycaproamide polyamide 6
- [CH 2 ] / [NHCO] 5.0
- polyethylene azide Pamid polyamide 26
- polytetramethylene succinamide polyamide 44
- [CH 2 ] / [NHCO] 3.0
- polytetramethylene glutamide Polyamide 45
- [CH 2 ] / [NHCO] 3.5
- polytetramethylene adipamide polyamide 46
- polytetramethylene azelamide polyamide 49
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups of the poly (dodecaneamide / caproamide) copolymer (polyamide 12/6) changes depending on the molar ratio of the constituent repeating units.
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups of polydodecane amide (polyamide 12) is 11.0, and the ratio of the number of methylene groups to the number of amide groups of polycaproamide (polyamide 6) [CH 2 ] / Since [NHCO] is 5.0, it can be calculated if the molar ratio of the constituent repeating units is known, and the dodecane amide unit / caproamide unit is 80:20 (mass ratio), 69.7: 30.3 (molar).
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups is 11.
- the raw material monomer (repeating unit) forming an aliphatic polyamide having a ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups is one component, and the number of methylene groups relative to the number of amide groups is the ratio [CH 2] / raw monomer [NHCO] to form a 8.0 below aliphatic polyamide ratio amide groups methylene groups in the copolymer using several kinds of (repeating units) [CH 2] / [NHCO] can be calculated from the molar ratio of constituent repeating units and the ratio of the number of methylene groups of each polyamide to the number of amide groups [CH 2 ] / [NHCO], and the ratio of the number of methylene groups to the number of amide groups [CH 2 ] / [NHCO]
- the copolymer having a value of 8.0 or more is included in the polyamide (A1) of the present application.
- polyamide (A1) is a polyundecanamide (A1) from the viewpoint of economy, ease of availability, and sufficient mechanical properties, heat resistance, chemical resistance and other physical properties of the laminated tube to be obtained.
- the polyamide (A2) is a polyamide other than the polyamide (A1), which has an amide bond (-CONH-) in the main chain, and is a lactam which is a raw material monomer (repeating unit) forming an polyamide, It can be obtained by polymerizing or copolymerizing an acid or a diamine and a dicarboxylic acid by a known method such as melt polymerization, solution polymerization, and solid phase polymerization (hereinafter may be referred to as polyamide (A2)).
- the polyamide (A2) is at least one selected from the group consisting of alicyclic polyamides, semiaromatic polyamides, and aliphatic polyamides having a ratio of the number of methylene groups to the number of amide groups of [CH 2 ] / [NHCO] of less than 8.0. It is a species. Furthermore, the absolute value of the difference between the solubility parameter SP value of polyamide (A1) and polyamide (A2) [
- the solubility parameter SP value is a value determined by the formula of Fedors shown below, is a value represented by the square root of the molecular cohesive energy density, and the unit is a value at (MPa) 1/2 at 25 ° C.
- solubility parameter may be referred to as the SP value.
- the SP value described in the present specification is a value in which the unit is (MPa) 1/2 .
- Solubility parameter SP value of each polyamide (A1) mentioned as a preferred example is (unit: (MPa) 1/2 ), poêtcane amide (polyamide 11, SP value: 22.9), poly dodecane amide ( Polyamide 12, SP value: 22.5), polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1), polynonamethylene azelamide (polyamide 99, SP value: 24.
- polyamide 910, SP value: 23.8 polynona methylene decamide
- polyamide 912, SP value: 23.2 polynonamethylene dodecamide
- polyamide 1010, SP value: 23.5 polydecamethylene sebacamide
- polyamide 1012, SP value: 22.9 polydodecamethylene dodecamide
- polyamide 1 12, SP value: 22.5) and a.
- the absolute value of the difference of the solubility parameter SP value with the polyamide (A1) may be 1.8 or more and 5.5 or less (MPa) 1/2 , which is satisfied and the number of methylene groups
- polycaproamide polyamide 6, SP value: 26.
- polytetramethylene glutamide polyamide 45, SP value: 29.2
- polytetramethylene adipamide polyamide 46, SP value: 28.3
- polytetramethylene suberamide polyamide 48, SP value: 26.9
- polytetramethylene azelamide polyamide 49, SP value: 26.3)
- polytetramethylene sebacamide polyamide 410, SP value: 25) 7
- polytetramethylene dodecamide polyamide 412, SP value: 24.9)
- polypentamethylene succinamide polyamide 54, SP value: 29.2)
- polypentamethylene glutamide polyamide 55, SP value: 28.3
- polypentamethylene adipamide polyamide 56, SP value: 27.5
- polypentamethylene suberamide polyamide 58, SP value: 26.3
- polypentamethylene aceramide polypentamethylene sebacamide
- polyamide (A2) is suitably selected so that the absolute value of the difference of solubility parameter SP value with polyamide (A1) may be 1.8 or more and 5.5 or less (MPa) 1/2 .
- polyamides (A1) polydodecane amide (polyamide 12, SP value: 22.5) and polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) having the lowest solubility parameter SP value are selected.
- polypentamethylene dodecamide polyamide 512, SP value: 24.5
- polydodecamethylene glutamide polyamide 125, SP value: 24.
- the absolute value of the difference of the solubility parameter SP value from 5) is 2.0 (MPa) 1/2 and is within the specified range of the present application. Therefore, polydodecanedeamide (polyamide 12, SP value: 22.5) or polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) as the polyamide (A1) and polypentamethylene dodecaamide as the polyamide (A2) Combinations of polyamide (polyamide 512, SP value: 24.5) and polydodecamethylene glutamide (polyamide 125, SP value: 24.5) are within the specified range of the present application. On the other hand, polyhexamethylene dodecamide (polyamide 612, SP value: 24.
- polyamide 99, SP value: 24. 1 having the highest solubility parameter SP value among the polyamide (A1).
- polypentamethylene dodecamide polyamide 512, SP value: 24.5
- polydodecamethylene glutamide polyamide 125, SP
- the absolute value of the difference between the solubility parameter SP value and the value: 24.5) is 0.4 (MPa) 1/2 , which is outside the specified range of the present application. Therefore, as the polyamide (A1), polyhexamethylene dodecamide (polyamide 612, SP value: 24.
- solubility parameter SP value 25.9 (MPa) 1 It is necessary to select two or more polyamides (A2).
- polyamides (A1) polydodecane amide (polyamide 12, SP value: 22.5) and polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) having the lowest solubility parameter SP value
- the absolute value of the difference in solubility parameter SP value of polytetramethylene adipamide (polyamide 46, SP value: 28.3) having the highest solubility parameter SP value among the polyamide (A2) is It is 5.8 (MPa) 1/2 , which is outside the specified range of the present application.
- polydodecane amide polyamide 12, SP value: 22.5) or polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) as the polyamide (A1) and polytetramethylene azidate as the polyamide (A2)
- the combination of pamide (polyamide 46, SP value: 28.3) is outside the specified range of the present application, and as polyamido (A1), polydodecane amide (polyamide 12, SP value: 22.5) and polydodecamethylene dodecamide
- polyamide 1212, SP value: 22.5 is selected, in order for the absolute value of the difference of the solubility parameter SP value to be 5.5 (MPa) 1/2 or less, the solubility parameter SP value is It is necessary to select a polyamide (A2) of 28.0 (MPa) 1/2 or less.
- polyhexamethylene dodecamide polyamide 612, SP value: 24. 1 or polynona methylene aceramide (polyamide 99, SP value: 24. 1) having the highest solubility parameter SP value among the polyamide (A1).
- polyamidomethylene adipamide polyamide 46, SP value: 28.3 having the highest solubility parameter SP value among the polyamide (A2).
- the value is 4.2 (MPa) 1/2 and is within the specified range of the present application. Therefore, as the polyamide (A1), polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1) or polynonamethylene azelamide (polyamide 99, SP value: 24. 1) and polytetramer as the polyamide (A 2) The combination of methylene adipamide (polyamide 46, SP value: 28.3) is within the specified range of the present application.
- the polyamide (A2) is a polycaproamide (polyamide 6), a polyhexamethylene adipamide (polyamide 66), a polyhexa At least one homopolymer selected from the group consisting of methylene azelamide (polyamide 69) and polyhexamethylene sebacamide (polyamide 610), and / or a co-catalyst using several kinds of raw material monomers forming these Polymer or polycaproamide (polyamide 6), polyhexamethylene adipamide (polyamide 66), polyhexamethylene azelamide A raw material monomer forming at least one selected from the group consisting of polyamide 69) and polyhex
- polycaproamide polyamide 6
- polyhexamethylene adipamide polyamide 66
- polyhexamethylene azelamide polyamide 69
- polyhexamethylene sebacamide polyamide 610
- poly (caproamide / hexamethylene) Adipamide) copolymer polyamide 6/66
- poly (caproamide / hexamethylene aceramide) copolymer polyamide 6/69
- poly (caproamide / hexamethylene sebacamide) copolymer polyamide 6 / 610
- poly (caproamide / hexamethylene dodecamide) copolymer polyamide 6/612
- poly (caproamide / dodecane amide) copolymer polyamide 6/12
- poly (caproamide / hexamethylene adipamide / hexa) Methylene sebacamide) copolymer poly 6/66/610
- the solubility parameter SP value of poly (caproamide / hexamethylene adipamide) copolymer is the solubility of polycaproamide (polyamide 6) and polyhexamethylene adipamide (polyamide 66) Since the parameter SP value is 26.9 (MPa) 1/2 , the solubility parameter SP value is 26.9 (MPa) 1/2 regardless of the mass ratio and the molar ratio of the constituent repeating units.
- polyamides (A1) polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1) and polynona methylene aceramide (polyamide 99, SP value: 24.
- the SP value is 26.9 (MPa) 1/2 regardless of the mass ratio and the molar ratio of constituent repeating units of poly (caproamide / hexamethylene adipamide) copolymer (polyamide 6/66).
- the absolute value of the difference in solubility parameter SP value is 2.8 (MPa) 1/2 , which is within the specified range of the present application. Therefore, as the polyamide (A1), polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1) or polynonamethylene azelamide (polyamide 99, SP value: 24.
- the absolute value of the difference in solubility parameter SP value is 4.4 (MPa) 1/2 , which is within the specified range of the present application. Therefore, as the polyamide (A1), polydodecane amide (polyamide 12, SP value: 22.5) or polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) and the polyamide (A2), poly (caproamide / The combination of hexamethylene adipamide copolymer (polyamide 6/66, SP value: 26.9) is within the specified range of the present application.
- solubility parameter SP value of the poly (caproamide / hexamethylene sebacamide) copolymer (polyamide 6/610) which is the polyamide (A2) varies depending on the molar ratio of the constituent repeating units.
- Solubility parameter SP value of polycaproamide (polyamide 6) is 26.9 (MPa) 1/2 and solubility parameter SP value of polyhexamethylene sebacamide (polyamide 610) is 24.9 (MPa) 1 If the molar ratio of the repeating unit of the constitutional unit is known, it can be calculated, and the caproamide unit / hexamethylene sebacamide unit is 80:20 (mass ratio), 85.2: 14.8 (molar).
- polyamide 6/610 85.2 / 14.8 mol%
- it has the highest solubility parameter SP value among the aforementioned polyamide (A1)
- polyhexamethylene dodecamide polyamide 612, SP value: 24. 1
- polynona methylene aceramide polyamide 99, SP value: 24. 1
- the absolute value of the difference of the solubility parameter SP value is It is 2.5 (MPa) 1/2 and is within the specified range of the present application.
- polyamide (A1) polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1) or polynonamethylene azelamide (polyamide 99, SP value: 24. 1) and the polyamide (A 2)
- the lowest solubility parameter SP value among the above-mentioned polyamide (A1) In the case where polydodecane amide (polyamide 12, SP value: 22.5) or polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) having is selected, the absolute value of the difference in solubility parameter SP value is It is 4.1 (MPa) 1/2 and is within the specified range of the present application.
- polyamide (A1) polydodecane amide (polyamide 12, SP value: 22.5) or polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) and the polyamide (A2)
- the kaproamide unit / hexamethylene sebacamide unit is 30:70 (mass ratio), 38.1 / 61.9 (mass ratio).
- polyamide 6/610 38.1 / 61.9 mol%
- it has the highest solubility parameter SP value among the aforementioned polyamide (A1)
- polyhexamethylene dodecamide polyamide 612, SP value: 24. 1
- polynona methylene aceramide polyamide 99, SP value: 24. 1
- the absolute value of the difference of the solubility parameter SP value is It is 1.6 (MPa) 1/2 , which is outside the specified range of the present application.
- polyamide (A1) polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1) or polynonamethylene azelamide (polyamide 99, SP value: 24. 1) and the polyamide (A 2)
- the lowest solubility parameter SP value among the above-mentioned polyamide (A1) In the case where polydodecane amide (polyamide 12, SP value: 22.5) or polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) having is selected, the absolute value of the difference in solubility parameter SP value is It is 3.2 (MPa) 1/2 , which is within the specified range of the present application.
- solubility parameter SP value of the poly (caproamide / dodecane amide) copolymer (polyamide 6/12) which is the polyamide (A2) varies depending on the molar ratio of the constituent repeating units.
- Solubility parameter SP value of polycaproamide (polyamide 6) is 26.9 (MPa) 1/2 and solubility parameter SP value of polydodecane amide (polyamide 12) is 22.5 (MPa) 1/2
- the caproamide unit / dodecane amide unit is 80:20 (mass ratio) and 87.5: 12.5 (molar ratio).
- Polyhexamethylene having the highest solubility parameter SP value among the above-mentioned polyamides (A1) relative to this poly (caproamide / dodecane amide) copolymer (polyamide 6/12 87.5 / 12.5 mol%)
- dodecamide polyamide 612, SP value: 24. 1
- polynona methylene aceramide polyamide 99, SP value: 24. 1
- the absolute value of the difference in solubility parameter SP value is 2.3 (MPa) 1/2 , which is within the specified range of the present application.
- polyamide (A1) polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1) or polynonamethylene azelamide (polyamide 99, SP value: 24. 1) and the polyamide (A 2)
- polyamide 99, SP value: 24. 1 polynona methylene aceramide
- polyamide 99, SP value: 24. 1 polynona methylene aceramide
- the absolute value of the difference of the solubility parameter SP value is 1.6 (MPa) 1/2 , which is outside the specified range of the present application. Therefore, as the polyamide (A1), polyhexamethylene dodecamide (polyamide 612, SP value: 24. 1) or polynonamethylene azelamide (polyamide 99, SP value: 24. 1) and the polyamide (A 2)
- the polyamide (A2) in the case of cycloaliphatic polyamide or semi-aromatic polyamide the absolute value of the difference between the solubility parameter SP value of the polyamide (A1) is 1.8 to 5.5 (MPa) 1 And the unit of SP value is (MPa) 1/2 as an alicyclic polyamide or semiaromatic polyamide satisfying this, and polymetaxylylene glutamide (polyamide MXD5, SP value: 29.4) ), Polymethaxylylene adipamide (polyamide MXD6, SP value: 28.6), polytetramethylene terephthalamide (polyamide 4 T, SP value: 29.4), polytetramethylene isophtalamide (polyamide 4 I, SP value) : 29.4), polytetramethylene hexahydroterephthalamide (polyamide 4 T (H), SP value: 27.1), polypentamethyl.
- Terephthalamide (polyamide 5T, SP value: 28.6), polypentamethylene isophthalamide (polyamide 5I, SP value: 28.6), polypentamethylene hexahydroterephthalamide (polyamide 5T (H), SP value: 26 .4), polyhexamethylene terephthalamide (polyamide 6T, SP value: 27.8), polyhexamethylene isophthalamide (polyamide 6I, SP value: 27.8), polyhexamethylene hexahydroterephthalamide (polyamide) 6T (H), SP value: 25.9), poly (2-methylpentamethylene terephthalamide) (polyamide M5T, SP value: 28.0), poly (2-methylpentamethyleneisophthalamide) (polyamide M5I , SP value: 28.0), poly (2-methylpentamethylene hexahydroterephthalate) Co) using (polyamide M5T (H), SP value: 26.0) and / or several starting monomers
- the semiaromatic polyamide (B1) or the semiaromatic polyamide (B2) described later may be used as well. it can.
- polyamide (A2) is a polycaproamide (polyamide 6) from the viewpoint of sufficiently securing various properties such as availability, economy, mechanical properties of the obtained laminated tube, and chemical resistance.
- the solubility parameter SP value of the poly (hexamethylene terephthalamide / hexamethylene isophthalamide) copolymer (polyamide 6T / 6I) exemplified as the more preferable polyamide (A2) is polyhexamethylene terephthalamide (polyamide) Since the solubility parameter SP value of 6T) and polyhexamethylene isophthalamide (polyamide 6I) is 27.8 (MPa) 1/2 , regardless of the mass ratio and molar ratio of the constituent repeating units, the solubility parameter The SP value is 27.8 (MPa) 1/2 .
- polyamides (A1) polyhexamethylene dodecamide (polyamide 612, SP value: 24.
- solubility parameter SP value is 27.50 regardless of the mass ratio and the molar ratio of the constituent repeating units of poly (hexamethylene terephthalamide / hexamethylene isophthalamide) copolymer (polyamide 6T / 6I). Since it is 8 (MPa) 1/2 , the absolute value of the difference in solubility parameter SP value is 3.7 (MPa) 1/2 , which is within the specified range of the present application.
- poly (hexa) as the polyamide (A2)
- the combination of methylene terephthalamide / hexamethylene isophthalamide) copolymer (polyamide 6T / 6I, SP value: 27.8) is within the specified range of the present application.
- polyamide 1212 polydodecane amide
- polyamide 1212 SP value: 22.5
- polydodecamethylene dodecamide polyamide 1212, SP value: 22.5
- the SP value is 27.8 (MPa, regardless of the mass ratio and the molar ratio of constituent repeating units of poly (hexamethylene terephthalamide / hexamethylene isophthalamide) copolymer (polyamide 6T / 6I). Since it is 1/2 , the absolute value of the difference in solubility parameter SP value is 5.3 (MPa) 1/2 , which is within the specified range of the present application.
- polyamido (A1) poly (dodecaneamide) (polyamide 12, SP value: 22.5) or polydodecamethylene dodecamide (polyamide 1212, SP value: 22.5) and polyamido (A2), poly (hexamethylene)
- polyamide 6T / 6I, SP value: 27.8 poly(ethylene)
- polyamide (A1) and polyamide (A2) As a manufacturing apparatus of polyamide (A1) and polyamide (A2), a batch type reaction kettle, a single tank type or multi tank type continuous reaction apparatus, a tubular continuous reaction apparatus, a single screw type kneading extruder, a twin screw type kneading extruder, etc. Examples of known kneader / reactor extruders and the like are known polyamide manufacturing apparatuses.
- polymerization method polymerization can be repeated by repeating operations of normal pressure, reduced pressure, and pressure using known methods such as melt polymerization, solution polymerization, and solid phase polymerization. These polymerization methods can be used alone or in combination as appropriate.
- the relative viscosity of polyamides (A1) and (A2) measured under the conditions of 96% sulfuric acid, 1% polymer, and 25 ° C. in accordance with JIS K-6920 ensures the mechanical properties of the resulting laminated tube From the viewpoint of securing the desired formability of the laminated tube by setting the viscosity at the time of melting to an appropriate range, it is preferably 1.5 or more and 5.0 or less, and is 1.8 or more and 4.5 or less Is more preferred.
- the terminal amino group concentration per gram of each of the polyamide (A1) and the polyamide (A2) in the aliphatic polyamide composition (A) is [A] ( ⁇ eq / g), and the terminal carboxyl group concentration is [B] ( ⁇ eq / g) [A]> [B] +10 from the viewpoint of sufficiently obtaining the interlaminar adhesion with the semiaromatic polyamide composition (B) and the durability thereof.
- B] +15 is more preferable
- [A]> [B] +20 is more preferable.
- the terminal amino group concentration [A] ( ⁇ eq / g) can be measured by dissolving the polyamide in a phenol / methanol mixed solution and titrating with 0.05 N hydrochloric acid.
- the terminal carboxyl group concentration [B] ( ⁇ eq / g) can be measured by dissolving the polyamide in benzyl alcohol and titrating with a 0.05 N sodium hydroxide solution.
- the polyamide (A1) and the polyamide (A2) are produced by polymerizing or copolymerizing the polyamide raw material in the presence of amines by a known method such as melt polymerization, solution polymerization and solid phase polymerization. . Or it manufactures by melt-kneading in presence of amines after superposition
- amines can be added at any stage during polymerization, or after polymerization, at any stage during melt-kneading, but in consideration of the interlayer adhesiveness of the laminated tube, they are added at the stage of polymerization. Is preferred.
- the amines include monoamines, diamines, triamines and polyamines.
- carboxylic acids such as monocarboxylic acids, dicarboxylic acids and tricarboxylic acids may be added as long as they do not deviate from the above range of terminal group concentration conditions. These amines and carboxylic acids may be added simultaneously or separately. Moreover, 1 type or 2 types or more can be used for amines and carboxylic acids of the following illustration.
- monoamines to be added include methylamine, ethylamine, propylamine, butylamine, pentylamine, hexylamine, heptylamine, octylamine, 2-ethylhexylamine, nonylamine, decylamine, undecylamine, dodecylamine, tridecylamine
- Aliphatic monoamines such as tetradecylamine, pentadecylamine, hexadecylamine, octadecylamine, octadecylenamine, eicosylamine and docosylamine; alicyclic monoamines such as cyclohexylamine and methylcyclohexylamine; benzylamine, ⁇ - Aromatic monoamines such as phenylmethylamine; N, N-dimethylamine, N, N-diethylamine, N, N-dipropylamine, N, N
- diamine to be added examples include 1,2-ethanediamine, 1,3-propanediamine, 1,4-butanediamine, 1,5-pentanediamine, 1,6-hexanediamine, 1,7-heptanediamine 1,8-octanediamine, 1,9-nonanediamine, 1,10-decanediamine, 1,11-undecanediamine, 1,12-dodecanediamine, 1,13-tridecanediamine, 1,14-tetradecanediamine 1,15-Pentadecanediamine, 1,16-hexadecanediamine, 1,17-heptadecanediamine, 1,18-octadecanediamine, 2-methyl-1,5-pentanediamine, 3-methyl-1,5-pentanediamine , 2-Methyl-1,8-octanediamine, 2,2,4-trimethyl-1,6-hexane Aliphatic diamines such as amines, 2,4,4-trimethyl-1,6-hexanediamine, 5-methyl-1,9
- triamine to be added examples include 1,2,3-triaminopropane, 1,2,3-triamino-2-methylpropane, 1,2,4-triaminobutane, 1,2,3,4- Tetraminobutane, 1,3,5-triaminocyclohexane, 1,2,4-triaminocyclohexane, 1,2,3-triaminocyclohexane, 1,2,4,5-tetraminocyclohexane, 1,3,5- Triaminobenzene, 1,2,4-triaminobenzene, 1,2,3-triaminobenzene, 1,2,4,5-tetraminobenzene, 1,2,4-triaminonaphthalene, 2,5,7 And -triaminonaphthalene, 2,4,6-triaminopyridine, 1,2,7,8-tetraminonaphthalene, 1,4,5,8-tetraminonaphthalene and the like. One or more of these may be used.
- the polyamine to be added may be a compound having a plurality of primary amino groups (-NH 2 ) and / or secondary amino groups (-NH-), for example, polyalkyleneimines, polyalkylene polyamines, polyvinyl amines, Polyallylamine etc. are mentioned.
- the amino group with active hydrogen is the reactive point of the polyamine.
- Polyalkyleneimines are produced by, for example, a method of ionically polymerizing alkyleneimines such as ethyleneimine and / or propyleneimine, or by polymerizing an alkyl oxazoline and then partially or completely hydrolyzing the polymer .
- alkyleneimines such as ethyleneimine and / or propyleneimine
- polyalkylene polyamines include diethylenetriamine, triethylenetetramine, pentaethylenehexamine, and a reaction product of ethylenediamine and a polyfunctional compound.
- Polyvinylamine can be obtained, for example, by polymerizing N-vinylformamide to form poly (N-vinylformamide) and then partially or completely hydrolyzing the polymer with an acid such as hydrochloric acid.
- Polyallylamine is generally obtained by polymerizing the hydrochloride of allylamine monomer and then removing the hydrochloric acid. One or more of these may be used. Among these, polyalkylene
- polyalkyleneimine one or two kinds of alkyleneimine having 2 to 8 carbon atoms such as ethyleneimine, propyleneimine, 1,2-butyleneimine, 2,3-butyleneimine, 1,1-dimethylethyleneimine and the like
- ethyleneimine propyleneimine
- 1,2-butyleneimine 1,2-butyleneimine
- 2,3-butyleneimine 1,1-dimethylethyleneimine and the like
- homopolymers and / or copolymers obtained by polymerizing species or more according to a conventional method Among these, polyethylene imine is more preferable.
- Polyalkyleneimines are obtained by polymerizing a primary amine, a secondary amine, and a branched polyalkyleneimine containing a tertiary amine, or an alkyl oxazoline, which is obtained by ring-opening polymerization of the alkyleneimine as a raw material, and polymerizing this. It may be either a linear type polyalkyleneimine containing only a primary amine and a secondary amine obtained by reaction, or a three-dimensionally crosslinked structure.
- polyalkyleneimines are generally derived from the reactivity of the active hydrogen atom on the nitrogen atom contained, and in addition to the tertiary amino group, a primary amino group and / or a secondary amino group having an active hydrogen atom. It has (imino group).
- the number of nitrogen atoms in the polyalkyleneimine is not particularly limited, and is preferably 4 or more and 3,000, more preferably 8 or more and 1,500 or less, and still more preferably 11 or more and 500 or less.
- the number average molecular weight of the polyalkyleneimine is preferably 100 or more and 20,000 or less, more preferably 200 or more and 10,000 or less, and still more preferably 500 or more and 8,000 or less.
- carboxylic acids to be added acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthate, caprylic acid, caprylic acid, pelargonic acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, myristoleic acid, Aliphatic monocarboxylic acids such as palmitic acid, stearic acid, oleic acid, linoleic acid, arachic acid, behenic acid, erucic acid; alicyclic monocarboxylic acids such as cyclohexane carboxylic acid, methyl cyclohexane carboxylic acid; benzoic acid, toluic acid Malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, hexa
- the amount of the amine to be added is appropriately determined by a known method in consideration of the terminal amino group concentration, terminal carboxyl group concentration and relative viscosity of the polyamide (A1) and polyamide (A2) to be produced.
- the amount of addition of the amines is to obtain sufficient reactivity and to obtain a polyamide having a desired viscosity.
- the polyamide (A1) and the polyamide (A2) it is preferable to add a diamine and / or a polyamine at the time of polymerization in order to satisfy the end group concentration condition among the amines exemplified above, from the viewpoint of gel formation suppression It is more preferable to add at least one member selected from the group consisting of aliphatic diamines, alicyclic diamines, and polyalkyleneimines during polymerization.
- the aliphatic polyamide composition (A) contains an elastomeric polymer (A3) containing a structural unit derived from an unsaturated compound having a carboxyl group and / or an acid anhydride group (elastomer polymer (A3) and Sometimes called).
- elastomer polymer (A3) (ethylene and / or propylene) / ⁇ -olefin copolymer, (ethylene and / or propylene) / ( ⁇ , ⁇ -unsaturated carboxylic acid ester) copolymer
- aroma Group vinyl compound / conjugated diene compound block copolymers can be mentioned, and one or more of these can be used.
- the (ethylene and / or propylene) / ⁇ -olefin copolymer is a polymer obtained by copolymerizing ethylene and / or propylene and an ⁇ -olefin having 3 or more carbon atoms, and it is an ⁇ - (3 or more carbon atoms)
- olefin propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-undecene, 1-dodecene, 1-tridecene, 1-tetradecene, 1-pentadecene, 1-hexadecene, 1-heptadecene, 1-octadecene, 1-nonadecene, 1-eicosene, 3-methyl-1-butene, 3-methyl-1-pentene, 3-ethyl-1-pentene, 4- Methyl-1-pentene, 4-methyl-1-
- the (ethylene and / or propylene) / ( ⁇ , ⁇ -unsaturated carboxylic acid ester) copolymer has a weight obtained by copolymerizing ethylene and / or propylene with an ⁇ , ⁇ -unsaturated carboxylic acid ester monomer.
- ⁇ -unsaturated carboxylic acid ester monomers such as methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, propyl acrylate, propyl methacrylate, butyl acrylate, butyl methacrylate , Pentyl acrylate, pentyl methacrylate, hexyl acrylate, hexyl methacrylate, heptyl acrylate, heptyl methacrylate, octyl acrylate, octyl methacrylate, nonyl acrylate, nonyl methacrylate, decyl acrylate, decyl methacrylate, acrylic 2-ethylhexyl acid, metac Le 2-ethylhexyl acrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, monomethyl maleate, monomethyl itaconate, dimethyl
- the aromatic vinyl compound / conjugated diene compound block copolymer is a block copolymer composed of an aromatic vinyl compound polymer block and a conjugated diene compound polymer block, and is an aromatic vinyl compound polymer A block copolymer having at least one block and at least one conjugated diene compound-based polymer block is used. Further, in the block copolymer described above, the unsaturated bond in the conjugated diene compound polymer block may be hydrogenated.
- the aromatic vinyl compound polymer block is a polymer block mainly composed of units derived from an aromatic vinyl compound.
- an aromatic vinyl compound styrene, o-methylstyrene, m-methylstyrene, p-methylstyrene, 1,5-dimethylstyrene, 2,4-dimethylstyrene, vinyl naphthalene, vinyl anthracene, 4-propyl
- examples thereof include styrene, 4-cyclohexylstyrene, 4-dodecylstyrene, 2-ethyl-4-benzylstyrene, 4- (phenylbutyl) styrene and the like, and one or more of these can be used.
- the aromatic vinyl compound polymer block may optionally have a unit composed of a small amount of another unsaturated monomer.
- Conjugated diene compound polymer blocks include 1,3-butadiene, chloroprene, isoprene, 2,3-dimethyl-1,3-butadiene, 1,3-pentadiene, 4-methyl-1,3-pentadiene, 1,3 -A polymer block formed from one or more conjugated diene compounds such as hexadiene, and in the case of a hydrogenated aromatic vinyl compound / conjugated diene compound block copolymer, the conjugated diene compound polymer Some or all of the unsaturated bonds in the block are saturated by hydrogenation.
- the molecular structure of the aromatic vinyl compound / conjugated diene compound block copolymer and the hydrogenated product thereof may be linear, branched, radial or any combination thereof.
- one aromatic vinyl compound polymer block and one conjugated diene compound polymer block are linear as an aromatic vinyl compound / conjugated diene compound block copolymer and / or a hydrogenated substance thereof.
- aromatic vinyl compound polymer block-conjugated diene compound polymer block-aromatic vinyl compound polymer block in this order aromatic vinyl compound polymer block-conjugated diene compound polymer block-aromatic vinyl compound polymer block in this order
- one or more triblock copolymers and hydrogenated products thereof are used, and unhydrogenated or hydrogenated styrene / butadiene block copolymer, unhydrogenated or hydrogenated styrene / isoprene block copolymer are preferably used.
- Polymer unhydrogenated or hydrogenated styrene / butadiene / styrene block copolymer, unhydrogenated or hydrogenated styrene / isoprene / styrene block Click copolymer, non-hydrogenated or hydrogenated styrene / (ethylene / butadiene) / styrene block copolymer, non-hydrogenated or include hydrogenated styrene / (isoprene / butadiene) / styrene block copolymer.
- the unsaturated compound having a carboxyl group forming the constituent unit of the elastomeric polymer (A3) includes acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, crotonic acid, mesaconic acid, citraconic acid, glutaconic acid, cis ⁇ , ⁇ -unsaturated carboxylic acids such as -4-cyclohexene-1,2-dicarboxylic acid, endobicyclo- [2.2.1] -5-heptene-2,3-dicarboxylic acid, and metal salts of these carboxylic acids An acid is mentioned.
- unsaturated compounds having an acid anhydride group ⁇ such as maleic anhydride, itaconic anhydride, citraconic anhydride, endobicyclo- [2.2.1] -5-heptene-2,3-dicarboxylic acid anhydride, etc.
- dicarboxylic anhydrides having a ⁇ -unsaturated bond One or more of these may be used. Among these, dicarboxylic acid anhydrides having an ⁇ , ⁇ -unsaturated bond are preferable, and maleic anhydride and itaconic acid anhydride are more preferable.
- the carboxyl group and / or acid anhydride group concentration in the elastomeric polymer (A3) is sufficient to improve the low temperature impact resistance, the interlayer adhesion with the semiaromatic polyamide composition (B) described later, and the durability thereof.
- the fluidity of the aliphatic polyamide composition (A) to be obtained it is preferably 25 ⁇ eq / g to 200 ⁇ eq / g, and more preferably 50 ⁇ eq / g to 150 ⁇ eq / g.
- the concentration of the carboxyl group and / or acid anhydride group in the elastomer polymer (A3) can be measured using a sample solution prepared by dissolving the elastomer polymer in a toluene solution and further adding ethanol to give an indicator of phenolphthalein It can be measured by titration with 0.1 N KOH ethanol solution.
- Content of polyamide (A1) in aliphatic polyamide composition (A) is 40 mass% or more and 90 mass% or less with respect to 100 mass% of aliphatic polyamide composition (A), and 50 mass% or more and 86 It is preferable that it is mass% or less, and it is more preferable that they are 60 mass% or more and 84 mass% or less. If the content of the polyamide (A1) is less than the above value, the mechanical properties of the resulting laminated tube may be inferior, while if it exceeds the above value, the interlayer adhesion of the resulting laminated tube and its durability It may be inferior in sex.
- Content of polyamide (A2) in aliphatic polyamide composition (A) is 5 mass% or more and 30 mass% or less with respect to 100 mass% of aliphatic polyamide composition (A), and 7 mass% or more and 25 It is preferable that it is mass% or less, and it is more preferable that it is 8 mass% or more and 20 mass% or less. If the content of the polyamide (A2) is less than the above value, the interlayer adhesion of the resulting laminated tube and its durability may be poor, while if it exceeds the above value, the mechanical properties of the resulting laminated tube are obtained. Properties and chemical resistance may be poor.
- Content of the elastomer polymer (A3) in an aliphatic polyamide composition (A) is 5 mass% or more and 30 mass% or less with respect to 100 mass% of aliphatic polyamide composition (A), and 7 mass%
- the content is preferably 25% by mass or less, and more preferably 8% by mass to 20% by mass.
- the content of the elastomer polymer (A3) is less than the above value, the low temperature impact resistance, the interlayer adhesion and the durability of the resulting laminated tube may be poor, while on the other hand, when the above value is exceeded The mechanical properties of the resulting laminated tube and the flowability of the resulting aliphatic polyamide composition may be poor.
- the method of mixing the polyamide (A1) and the polyamide (A2) and the elastomer polymer (A3) is not particularly limited, and various additives may be blended as necessary to adopt various methods conventionally known.
- Can. a method of uniformly dry blending the pellets of polyamide (A1), polyamide (A2), and elastomer polymer (A3) with each other using a tumbler or a mixer so as to achieve the above mixing ratio, both are required
- It can be manufactured by, for example, a method of dry-blending in advance at a concentration used at the time of molding, and melt-kneading with other components added according to the above. Melt-kneading can be performed using kneaders, such as a single-screw extruder, a twin-screw extruder, a kneader, and a Banbury mixer.
- the aliphatic polyamide composition (A) may be a mixture with other thermoplastic resin.
- the total content of the polyamide (A1), the polyamide (A2) and the elastomeric polymer (A3) in the aliphatic polyamide composition (A) is preferably 80% by mass or more and 90% by mass or more More preferable.
- thermoplastic resins to be mixed high density polyethylene (HDPE), medium density polyethylene (MDPE), low density polyethylene (LDPE), linear low density polyethylene (LLDPE), ultra high molecular weight polyethylene (UHMWPE) , Polypropylene (PP), polybutene (PB), polymethylpentene (TPX), ethylene / propylene copolymer (EPR), ethylene / butene copolymer (EBR), ethylene / vinyl acetate copolymer (EVA), ethylene / Acrylic acid copolymer (EAA), ethylene / methacrylic acid copolymer (EMAA), ethylene / methyl acrylate copolymer (EMA), ethylene / methyl methacrylate copolymer (EMMA), ethylene / ethyl acrylate Polyolefin resin such as copolymer (EEA); poly Tyrene (PS), Syndiotactic Polystyrene (SPS), Methyl Methacrylate
- Polyolefin resin and polystyrene resin Poly Tylene terephthalate (PBT), polyethylene terephthalate (PET), polyethylene isophthalate (PEI), poly (ethylene terephthalate / ethylene isophthalate) copolymer (PET / PEI), polytrimethylene terephthalate (PTT), polycyclohexanedimethylene terephthalate (PCT), polyester resins such as polyethylene naphthalate (PEN), polybutylene naphthalate (PBN), polyarylate (PAR), liquid crystal polyester (LCP), polylactic acid (PLA), polyglycolic acid (PGA); polyacetal (POM), polyether resins such as polyphenylene ether (PPO); polysulfone (PSU), polysulfone (PESU), polyphenylsulfone (PPSU) etc Phone resins; polythioether resins such as polyphenylene sulfide (PPS), polythioether sulfone
- Thermoplastic polyurethane resins polyamide elastomers, polyurethane elastomers Mer, polyester elastomer, etc., and in some cases polyvinylidene fluoride (PVDF), polyvinyl fluoride (PVF), polytetrafluoroethylene (PTFE), polytetrafluoroethylene (PCTFE), tetrafluoroethylene / ethylene copolymer (ETFE), ethylene / chlorotrifluoroethylene copolymer (ECTFE), tetrafluoroethylene / hexafluoropropylene copolymer (FEP), tetrafluoroethylene / hexafluoropropylene / vinylidene fluoride copolymer (THV), tetramer Fluoroethylene / hexafluoropropylene / vinylidene fluoride / perfluoro (alkyl vinyl ether) copolymer, tetrafluoro
- an antioxidant if necessary, an antioxidant, a heat stabilizer, an ultraviolet light absorber, a light stabilizer, a lubricant, an inorganic filler, an antistatic agent, a flame retardant, and crystallization.
- An accelerator, a coloring agent, etc. may be added.
- the (b) layer of the laminated tube contains the semiaromatic polyamide composition (B).
- the semiaromatic polyamide composition (B) comprises a semiaromatic polyamide (B1) or a semiaromatic polyamide (B2), and in the semiaromatic polyamide composition (B), the semiaromatic polyamide (B1) Or 60% by mass or more of the semiaromatic polyamide (B2), and the semiaromatic polyamide (B1) is an aliphatic diamine having 9 or 10 carbon atoms with respect to all diamine units of the aromatic polyamide (B1)
- the semiaromatic polyamide (B2) contains 50 mol% or more of units and contains 50 mol% or more of terephthalic acid units and / or naphthalenedicarboxylic acid units with respect to all the dicarboxylic acid units of the semiaromatic polyamide (B1) Containing 50 mol% or more of xylylene diamine units
- the semi-aromatic polyamide composition (B) has an aspect including a semi-aromatic polyamide (B1) (hereinafter sometimes referred to as semi-aromatic polyamide (B1)), and the semi-aromatic polyamide (B1) A diamine unit containing 50 mol% or more of an aliphatic diamine unit having 9 or 10 carbon atoms based on all diamine units of the semiaromatic polyamide (B1) and all dicarboxylic acid units of the semiaromatic polyamide (B1) It contains a dicarboxylic acid unit containing 50% by mole or more of a terephthalic acid unit and / or a naphthalene dicarboxylic acid unit.
- the content of the aliphatic diamine unit having 9 or 10 carbon atoms in the semi-aromatic polyamide (B1) is sufficient for various physical properties such as heat resistance, chemical resistance, impact resistance, and chemical liquid barrier property of the obtained laminated tube From the viewpoint of ensuring the above, it is 50 mol% or more, preferably 55 mol% or more, and more preferably 60 mol% or more with respect to all diamine units of the semiaromatic polyamide (B1).
- Examples of the aliphatic diamine unit having 9 or 10 carbon atoms include units derived from 1,9-nonanediamine, 1,10-decanediamine and the like. As long as the number of carbon atoms satisfies the above, 2,2,4-trimethyl-1,6-hexanediamine, 2,4,4-trimethyl-1,6-hexanediamine, 2,4-diethyl-1,6-hexane Diamine, 2,2-dimethyl-heptanediamine, 2,3-dimethyl-heptanediamine, 2,4-dimethyl-heptanediamine, 2,5-dimethyl-heptanediamine, 2-methyl-1,8-octanediamine, 3 -Methyl-1,8-octanediamine, 4-methyl-1,8-octanediamine, 1,3-dimethyl-1,8-octanediamine, 1,4-dimethyl-1,8-octanediamine, 2,2 -Dimethyl-1,8-oct
- 1,9-nonanediamine, 2-methyl-1,8-octanediamine, 1,10-decanediamine Units which are derived are preferred.
- the molar ratio of 1,9-nonanediamine unit to 2-methyl-1,8-octanediamine unit is the formability and resistance From the viewpoint of the balance of impact properties, it is preferably 30: 70 mol% or more and 98: 2 mol% or less, and more preferably 40: 60 mol% or more and 95: 5 mol% or less.
- the diamine units in the semi-aromatic polyamide (B1) contain other diamine units other than aliphatic diamine units having 9 or 10 carbon atoms, as long as the excellent properties of the resulting laminated tube are not impaired. It may be.
- Other diamine units include 1,2-ethanediamine, 1,3-propanediamine, 1,4-butanediamine, 1,5-pentanediamine, 1,6-hexanediamine, 1,7-heptanemethane, 1 , 8-octanediamine, 1,11-undecanediamine, 1,12-dodecanediamine, 1,13-tridecanediamine, 2-methyl-1,5-pentanediamine, 3-methyl-1,5-pentanediamine, etc.
- Units derived from aliphatic diamines 1,3-cyclohexanediamine, 1,4-cyclohexanediamine, 1,3-bis (aminomethyl) cyclohexane, 1,4-bis (aminomethyl) cyclohexane, bis (4- (4) Aminocyclohexyl) methane, 2,2-bis (4-aminocyclohexyl) propane, bis (3-methyl-4) Aminocyclohexyl) methane, 2,2-bis (3-methyl-4-aminocyclohexyl) propane, 5-amino-2,2,4-trimethyl-1-cyclopentanemethylamine, 5-amino-1,3,3 -Trimethylcyclohexanemethylamine, bis (aminopropyl) piperazine, bis (aminoethyl) piperazine, 2,5-bis (aminomethyl) norbornane, 2,6-bis (aminomethyl) norbornane, 3,8-bis (aminomethyl
- the content of the terephthalic acid unit and / or the naphthalenedicarboxylic acid unit in the semiaromatic polyamide (B1) sufficiently secures various properties such as heat resistance, chemical resistance and chemical liquid barrier property of the obtained laminated tube From the viewpoint, it is 50 mol% or more, preferably 55 mol% or more, and more preferably 60 mol% or more based on all dicarboxylic acid units of the semiaromatic polyamide (B1).
- naphthalene dicarboxylic acid unit examples include units derived from 2,6-naphthalene dicarboxylic acid, 2,7-naphthalene dicarboxylic acid, 1,4-naphthalene dicarboxylic acid, 1,5-naphthalene dicarboxylic acid and the like. One or more of these may be used.
- naphthalenedicarboxylic acid units units derived from 2,6-naphthalenedicarboxylic acid and 2,7-naphthalenedicarboxylic acid are preferable in consideration of economy and ease of availability.
- the dicarboxylic acid unit in the semi-aromatic polyamide (B1) may be any other dicarboxylic acid unit other than terephthalic acid unit and / or naphthalene dicarboxylic acid unit, as long as the excellent properties of the resulting laminated tube are not impaired. May be included.
- dicarboxylic acid units include malonic acid, dimethylmalonic acid, succinic acid, glutaric acid, adipic acid, 2-methyl adipic acid, pimelic acid, 2,2-dimethyl glutaric acid, 2,2-diethyl succinic acid, suberin Acid, azelaic acid, 2,2,4-trimethyladipic acid, 2,4,4-trimethyladipic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid Unit derived from aliphatic dicarboxylic acid such as acid, octadecanedioic acid, eicosane diacid, etc .; Alicyclic such as 1,3-cyclopentane dicarboxylic acid, 1,3-cyclohexane dicarboxylic acid, 1,
- units derived from aromatic dicarboxylic acids are preferred.
- the content of these other dicarboxylic acid units is less than 50 mol%, preferably 45 mol% or less, and 40 mol% or less, based on the total dicarboxylic acid units of the semiaromatic polyamide (B1). Is more preferred.
- polyvalent carboxylic acids such as trimellitic acid, trimesic acid and pyromellitic acid can also be used within the range where melt molding is possible.
- the semiaromatic polyamide (B1) may contain other units other than the dicarboxylic acid unit and the diamine unit, as long as the excellent properties of the resulting laminated tube are not impaired.
- Other units include units derived from lactams such as caprolactam, enanthate lactam, undecane lactam, dodecane lactam, ⁇ -pyrrolidone, and ⁇ -piperidone; 6-aminocaproic acid, 7-aminoheptanoic acid, 9-aminononanoic acid, 11 -Aliphatic aminocarboxylic acids such as -aminoundecanoic acid and 12-aminododecanoic acid; and units derived from aminocarboxylic acids of aromatic aminocarboxylic acids such as p-aminomethylbenzoic acid.
- the content of the other units is preferably 45 mol% or less, more preferably 40 mol% or less, and 35 mol% or less based on all dicarboxylic acid units of the semiaromatic polyamide (B1). It is further preferred that
- a production apparatus for the semiaromatic polyamide (B1) a batch reaction kettle, a single tank or multi-tank continuous reaction apparatus, a tubular continuous reaction apparatus, a single screw type kneading extruder, a twin screw type kneading extruder
- kneader / reactor extruders and the like are known polyamide manufacturing apparatuses.
- polymerization method polymerization can be repeated by repeating operations of normal pressure, reduced pressure, and pressure using known methods such as melt polymerization, solution polymerization, and solid phase polymerization. These polymerization methods can be used alone or in combination as appropriate.
- phosphoric acid, phosphorous acid, hypophosphorous acid, salts or esters thereof and the like can be added as a catalyst.
- phosphorous acid or hypophosphorous acid for example, phosphoric acid, phosphorous acid or hypophosphorous acid and potassium, sodium, magnesium, vanadium, calcium, zinc, cobalt, manganese, tin ,
- Metal salts such as tungsten, germanium, titanium and antimony, ammonium salts of phosphoric acid, phosphorous acid or hypophosphorous acid, ethyl esters of phosphoric acid, phosphorous acid or hypophosphorous acid, isopropyl ester, butyl ester Hexyl ester, isodecyl ester, decyl ester, stearyl ester, phenyl ester and the like. One or more of these may be used.
- the semi-aromatic polyamide composition (B) has an aspect including a semi-aromatic polyamide (B2) (hereinafter sometimes referred to as semi-aromatic polyamide (B2)), and the semi-aromatic polyamide (B2)
- B2 a semi-aromatic polyamide
- B2 A diamine unit containing 50 mol% or more of a xylylene diamine unit and / or a bis (aminomethyl) naphthalene unit with respect to all the diamine units of the semiaromatic polyamide (B2) It contains a dicarboxylic acid unit containing 50 mol% or more of an aliphatic dicarboxylic acid unit having 9 or 10 carbon atoms, based on the unit.
- the content of the xylylenediamine unit and / or the bis (aminomethyl) naphthalene unit in the semi-aromatic polyamide (B2) is different from the heat resistance, the chemical resistance, the impact resistance, the chemical liquid barrier property etc From the viewpoint of sufficiently securing physical properties, it is 50 mol% or more, preferably 55 mol% or more, and more preferably 60 mol% or more based on all diamine units of the semiaromatic polyamide (B2). preferable.
- xylylenediamine units include units derived from o-xylylenediamine, m-xylylenediamine, and p-xylylenediamine. One or more of these may be used. Among the above-mentioned xylylene diamine units, units derived from m-xylylene diamine and p-xylylene diamine are preferable.
- bis (aminomethyl) naphthalene units 1,4-bis (aminomethyl) naphthalene, 1,5-bis (aminomethyl) naphthalene, 2,6-bis (aminomethyl) naphthalene, 2,7-bis (amino And units derived from methyl) naphthalene and the like. One or more of these may be used.
- the bis (aminomethyl) naphthalene units units derived from 1,5-bis (aminomethyl) naphthalene and 2,6-bis (aminomethyl) naphthalene are preferable.
- the diamine unit in the semi-aromatic polyamide (B2) is within the range not to impair the excellent properties of the resulting laminated tube, other diamines other than xylylene diamine unit and / or bis (aminomethyl) naphthalene unit It may contain units.
- diamine units include 1,2-ethanediamine, 1,3-propanediamine, 1,4-butanediamine, 1,5-pentanediamine, 1,6-hexanediamine, 1,7-heptanediamine, 1 , 8-octanediamine, 1,9-nonanediamine, 1,10-decanediamine, 1,11-undecanediamine, 1,12-dodecanediamine, 1,13-tridecanediamine, 1,14-tetradecanediamine, 1, 15-pentadecanediamine, 1,16-hexadecanediamine, 1,17-heptadecanediamine, 1,18-octadecanediamine, 1,19-nonadecanediamine, 1,20-eicosane diamine, 2-methyl-1,5 -Pentanediamine, 3-methyl-1,5-pentanediamine, 2-methyl-1,8-octane Derived from aliphatic diamines such as amines, 2,2,4-trimethyl-1,6-hexanedia
- One or more of these may be used.
- units derived from aromatic diamines are preferred.
- the content of these other diamine units is less than 50 mol%, preferably 45 mol% or less, and preferably 40 mol% or less based on all diamine units of the semiaromatic polyamide (B2). More preferable.
- Examples of the aliphatic dicarboxylic acid unit having 9 or 10 carbon atoms include units derived from azelaic acid, sebacic acid and the like. As long as the number of carbon atoms satisfies the above, it may contain a unit derived from a branched aliphatic dicarboxylic acid such as 2,2,4-trimethyladipic acid or 2,4,4-trimethyladipic acid. . One or more of these may be used. Among the aliphatic dicarboxylic acid units having 9 or 10 carbon atoms, units derived from 1 sebacic acid are preferable from the viewpoint of availability and economy.
- the content of the aliphatic dicarboxylic acid unit having 9 or 10 carbon atoms in the semi-aromatic polyamide (B2) is sufficient to satisfy various physical properties such as heat resistance, chemical resistance and chemical liquid barrier property of the obtained laminated tube From the viewpoint of securing, it is 50 mol% or more, preferably 55 mol% or more, and more preferably 60 mol% or more based on all dicarboxylic acid units of the semiaromatic polyamide (B2).
- the dicarboxylic acid unit in the semi-aromatic polyamide (B2) is a dicarboxylic acid other than the aliphatic dicarboxylic acid unit having an atomic number of 9 or 10, as long as the excellent properties of the resulting laminated tube are not impaired. It may contain units.
- dicarboxylic acid units include malonic acid, dimethylmalonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, Units derived from aliphatic dicarboxylic acids such as hexadecanedioic acid, octadecanedioic acid, eicosane diacid, 2-methyladipic acid, 2,2-dimethylglutaric acid, 2,2-diethylsuccinic acid, 2-butylsuberic acid and the like Units derived from alicyclic dicarboxylic acids such as 1,3-cyclopentane dicarboxylic acid, 1,3-cyclohexane dicarboxylic acid, 1,4-cyclohexane dicarboxylic acid
- terephthalic acid isophthalic acid, 1,4-naphthalene dicarboxylic acid Acid, 1,5-naphthalenedicarboxylic acid, 2,6-naphthalenedicarboxylic acid, 2,7 Naphthalene dicarboxylic acid, 1,3-phenylenedioxydiacetic acid, 1,4-phenylenedioxydiacetic acid, 4,4'-oxydibenzoic acid, diphenylmethane-4,4'-dicarboxylic acid, diphenylethane-4,4 ' -Dicarboxylic acid, diphenylpropane-4,4'-dicarboxylic acid, diphenylether-4,4'-dicarboxylic acid, diphenylsulfone-4,4'-dicarboxylic acid, 4,4'-biphenyldicarboxylic acid, 4,4'- The unit derived from aromatic dicarboxylic acids, such as triphenyl dicarboxylic acid, is mentioned
- the content of these other dicarboxylic acid units is less than 50 mol%, preferably 45 mol% or less, and 40 mol% or less based on all dicarboxylic acid units of the semiaromatic polyamide (B2). Is more preferred.
- polyvalent carboxylic acids such as trimellitic acid, trimesic acid and pyromellitic acid can also be used within the range where melt molding is possible.
- the semiaromatic polyamide (B2) may contain other units other than the dicarboxylic acid unit and the diamine unit, as long as the excellent properties of the resulting laminated tube are not impaired.
- Other units include units derived from lactams such as caprolactam, enanthate lactam, undecane lactam, dodecane lactam, ⁇ -pyrrolidone, and ⁇ -piperidone; 6-aminocaproic acid, 7-aminoheptanoic acid, 9-aminononanoic acid, 11 -Aliphatic aminocarboxylic acids such as -aminoundecanoic acid and 12-aminododecanoic acid; and units derived from aminocarboxylic acids of aromatic aminocarboxylic acids such as p-aminomethylbenzoic acid.
- the content of the other units is preferably 45 mol% or less, more preferably 40 mol% or less, and 35 mol% or less based on all dicarboxylic acid units of the semiaromatic polyamide (B2). It is further preferred that
- the apparatus for producing the semi-aromatic polyamide (B2) may be a batch reaction kettle, a single tank or multi-tank continuous reaction apparatus, a tubular continuous reaction apparatus, a single-screw kneading extruder, a twin-screw kneading extruder, etc.
- Well-known polyamide manufacturing apparatuses, such as a reaction extruder are mentioned.
- As a method for producing the semiaromatic polyamide (B2) there are known methods such as melt polymerization, solution polymerization and solid phase polymerization, and using these methods, normal pressure, pressure reduction, pressurization operation is repeated to make semi-aromatic Group polyamide (B2) can be produced.
- melt polymerization method is preferable.
- a nylon salt consisting of xylylenediamine and / or bis (aminomethyl) naphthalene and an aliphatic dicarboxylic acid having 9 or 10 carbon atoms is pressurized, heated, and added with water and condensed water in the presence of water. It is manufactured by the method of polymerizing in a molten state, excluding.
- xylylenediamine and / or bis (aminomethyl) naphthalene is directly added to a molten aliphatic dicarboxylic acid having 9 or 10 carbon atoms and subjected to polycondensation under normal pressure.
- xylylenediamine and / or bis (aminomethyl) naphthalene are continuously added to the aliphatic dicarboxylic acid having 9 or 10 carbon atoms, during which time the reaction system The polymerization proceeds while raising the temperature of the reaction system so that the temperature is equal to or higher than the melting point of the generated oligoamide and polyamide.
- the semiaromatic polyamide (B2) may be subjected to solid phase polymerization after being produced by a melt polymerization method.
- a phosphorus atom-containing compound can be added as a catalyst or to enhance processing stability during melt molding and to prevent coloration.
- a phosphorus atom containing compound hypophosphorous acid, phosphorous acid, phosphoric acid, pyrophosphoric acid, metaphosphoric acid, phosphonous acid phosphonic acid and derivatives thereof, alkaline earth metal salts of hypophosphorous acid, phosphorous acid Alkali metal salt, alkaline earth metal salt of phosphorous acid, alkali metal salt of phosphoric acid, alkaline earth metal salt of phosphoric acid, alkali metal salt of pyrophosphoric acid, alkaline earth metal salt of pyrophosphoric acid, alkali of metaphosphoric acid Metal salts, alkaline earth metal salts of metaphosphoric acid, alkali metal salts of phosphonous acid, alkaline earth metal salts of phosphonous acid, alkali metal salts of phosphonic acid, and alkaline earth metal salts of phosphonic acid
- phosphinic acid hypophosphorous acid
- ethyl hypophosphite dimethylphosphinic acid, phenylmethylphosphinic acid, sodium hypophosphite, potassium hypophosphite, lithium hypophosphite, Calcium phosphite, magnesium hypophosphite, phosphorous acid, triethyl phosphite, triphenyl phosphite, sodium phosphite, sodium hydrogen phosphite, potassium phosphite, potassium hydrogen phosphite, lithium phosphite , Lithium hydrogen phosphite, magnesium phosphite, magnesium hydrogen phosphite, calcium phosphite, calcium hydrogen phosphite, pyrophosphite, phosphoric acid, sodium phosphate, sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate , Potassium
- these phosphorus atom containing compounds may be a hydrate.
- the content of the phosphorus atom-containing compound is a phosphorus atom concentration relative to 100 parts by mass of the semiaromatic polyamide (B2) from the viewpoint of sufficient catalytic effect during polymerization, sufficient securing of the color prevention effect, and suppression of gel generation. It is preferable that it is 0.030 mass part or more and 0.30 mass part or less in conversion, It is more preferable that it is 0.050 mass part or more and 0.20 mass part or less, 0.070 mass part or more and 0.15 mass part It is more preferable that it is the following.
- These phosphorus atom-containing compounds are added to the nylon salt aqueous solution which is a raw material of the semi-aromatic polyamide (B2), a method of adding to diamine or dicarboxylic acid, a method of adding to dicarboxylic acid in molten state, during melt polymerization
- the method of adding etc. is mentioned, as long as it can disperse
- An alkali metal compound or an alkaline earth metal compound can be added to the semiaromatic polyamide (B2) in combination with the phosphorus atom-containing compound.
- an alkali metal compound or an alkaline earth metal compound is also present.
- alkali metal compound an alkali metal hydroxide, an alkaline earth metal hydroxide, an alkali metal acetate, an alkaline earth metal acetate, an alkali metal / alkaline earth metal carbonate, and an alkali metal / alkaline earth metal Alkoxides are mentioned, alkali metal hydroxides and / or alkali metal acetates being preferred.
- an alkali metal / alkaline earth metal such as lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, magnesium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide and the like Hydroxides; lithium acetate, sodium acetate, potassium acetate, rubidium acetate, cesium acetate, magnesium acetate, calcium acetate, calcium acetate, strontium acetate, barium acetate alkali metal / alkaline earth metal acetate; lithium carbonate, sodium carbonate, Alkali metal / alkaline earth metal carbonates such as potassium carbonate, rubidium carbonate, cesium carbonate, magnesium carbonate, calcium carbonate, strontium carbonate and barium carbonate; sodium methoxide, sodium ethoxide, sodium propoxide Sodium butoxide, potassium methoxide, lithium methoxide, magnesium methoxide, alkoxides of an alkali metal compound
- the value obtained by dividing the number of moles of the compound by the number of moles of phosphorus atom containing compound converted is It is preferable that it is 0.30 or more and 2.0 or less, more preferably 0.40 or more and 1.9 or less, and more preferably 0.50 or more and 1.8 or less, from the viewpoint of the balance between acceleration and suppression of the amidification reaction.
- the addition method of these alkali metal compounds or alkaline earth metal compounds is a method of adding to an aqueous solution of nylon salt which is a raw material of semi-aromatic polyamide (B2), a diamine or a dicarboxylic acid, or a method of adding to a dicarboxylic acid in a molten state.
- nylon salt which is a raw material of semi-aromatic polyamide (B2), a diamine or a dicarboxylic acid, or a method of adding to a dicarboxylic acid in a molten state.
- the relative viscosity of the semi-aromatic polyamide (B1) and the semi-aromatic polyamide (B2) measured under the conditions of 96% sulfuric acid, 1% of polymer concentration, and 25 ° C. in accordance with JIS K-6920 is the obtained laminated tube
- it is preferably 1.8 or more and 3 or more. .5 or less is more preferable, and 2.0 or more and 3.0 or less is more preferable.
- One or two or more of monoamines, diamines, polyamines, monocarboxylic acids and dicarboxylic acids can be added as appropriate in combination for molecular weight control and melt stabilization during molding processing.
- aliphatic monoamines such as methylamine, ethylamine, propylamine, butylamine, hexylamine, octylamine, decylamine, stearylamine, dimethylamine, diethylamine, dipropylamine and dibutylamine; alicyclic amines such as cyclohexylamine and dicyclohexylamine Monoamines; Aromatic monoamines such as aniline, toluidine, diphenylamine and naphthylamine; 1,4-butanediamine, 1,5-pentanediamine, 1,6-hexanediamine, 1,8-octanediamine, 2-methyl-1,5 Aliphatic diamines such as pentanediamine; alicyclic diamines such as cyclohexanediamine, bis (aminomethyl) cyclohexane, 5-amino-1,3,3-trimethylcyclohexanemethylamine; m-pheny Aromatic di
- the amount of the molecular weight modifier to be used varies depending on the reactivity of the molecular weight modifier and the polymerization conditions, but it is appropriately determined so that the relative viscosity of the polyamide to be finally obtained is in the above range.
- the ends of the molecular chains of the semiaromatic polyamide (B1) and the semiaromatic polyamide (B2) are sealed with an end capping agent, and 10% or more of the end groups are sealed. It is more preferable that it be stopped, and it is further preferable that 20% or more of the end groups are sealed.
- the end capping agent is not particularly limited as long as it is a monofunctional compound having reactivity with the amino group or carboxyl group at the polyamide end, but from the viewpoint of reactivity, stability of the sealing end, etc.
- An acid or a monoamine is preferred, and a monocarboxylic acid is more preferred from the viewpoint of ease of handling and the like.
- acid anhydrides such as phthalic anhydride, monoisocyanates, mono acid halides, monoesters, monoalcohols and the like can also be used.
- the monocarboxylic acid used as the end capping agent is not particularly limited as long as it has reactivity with an amino group, but the above-mentioned aliphatic monocarboxylic acid, alicyclic monocarboxylic acid and aromatic monocarboxylic acid may be used. Carboxylic acid etc. are mentioned. Among these, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, caprylic acid, lauric acid, tridecylic acid, myristic acid, palmitic acid, stearic acid from the viewpoints of reactivity, stability of sealing end, price, etc. And benzoic acid are preferred.
- the monoamine used as the end capping agent is not particularly limited as long as it has reactivity with a carboxyl group, and the above-mentioned aliphatic monoamines, alicyclic monoamines, aromatic monoamines and the like can be mentioned.
- butylamine, hexylamine, octylamine, decylamine, stearylamine, cyclohexylamine and aniline are preferable from the viewpoint of reactivity, boiling point, stability of sealing end, price and the like.
- the amount of the end capping agent used can be appropriately selected in consideration of the reactivity of the end capping agent used, the boiling point, the reaction apparatus, the reaction conditions, and the like. From the viewpoint of adjusting the degree of polymerization, it is preferably 0.1 mol% or more and 15 mol% or less with respect to the total number of moles of the dicarboxylic acid and the diamine which are raw material components.
- An impact modifier is preferably added to the semiaromatic polyamide composition (B) in order to improve the low temperature impact resistance of the semiaromatic polyamide (B1) and the semiaromatic polyamide (B2). It is more preferable to add the elastomer polymer (A3) containing the structural unit derived from the unsaturated compound having a carboxyl group and / or an acid anhydride group described in the aliphatic polyamide composition (A) . If the elastomeric polymer (A3) does not have a carboxyl group and / or an acid anhydride group, the impact improving effect may be insufficient.
- the content of the impact modifier is preferably 100 parts by mass of the main component semi-aromatic polyamide (B1) or semi-aromatic polyamide (B2) from the viewpoint of sufficiently securing the mechanical strength and low-temperature impact resistance of the laminated tube.
- the amount is preferably 1 to 30 parts by mass, and more preferably 3 to 25 parts by mass.
- the semiaromatic polyamide composition (B) may contain other thermoplastic resins together with the semiaromatic polyamide (B1) or the semiaromatic polyamide (B2).
- the resin similar to the case of the said aliphatic polyamide composition (A) is mentioned.
- it may be a mixture with polyamide (A1) and / or polyamide (A2).
- the content of the semiaromatic polyamide (B1) or the semiaromatic polyamide (B2) in the semiaromatic polyamide composition (B) is 60% by mass or more, preferably 70% by mass or more.
- polyamide (A2) is semi-aromatic polyamide (B1) or semi-aromatic polyamide (B2)
- a conductive filler an antioxidant, a heat stabilizer, an ultraviolet light absorber, a light stabilizer, a lubricant, an inorganic filler, an antistatic agent, A flame retardant, a crystallization accelerator, a plasticizer, a colorant, a lubricant and the like may be added.
- the laminated tube preferably further has a (c) layer.
- a fluorine-containing polymer (C) hereinafter referred to as a fluorine-containing polymer (C) in which a functional group having reactivity with amino groups is introduced into the molecular chain There is.
- the fluorine-containing polymer (C) is a fluorine-containing polymer in which a functional group having reactivity to an amino group is introduced into a molecular chain.
- the fluorine-containing polymer (C) is a polymer (homopolymer or copolymer) having a repeating unit derived from at least one fluorine-containing monomer. It is not particularly limited as long as it is a heat-melt processable fluorine-containing polymer.
- TFE tetrafluoroethylene
- VDF vinylidene fluoride
- VF vinyl fluoride
- CTFE chlorotrifluoroethylene
- N in the compound represented by is from the viewpoint of securing the effect of modifying the fluorine-containing polymer (for example, suppressing the formation of a crack in forming a copolymer or in a molded product) and obtaining sufficient polymerization reactivity , Is an integer of 2 or more and 10 or less.
- n in the formula is more preferably 2 or more and 4 or less.
- the fluorine-containing polymer (C) may further contain a polymerization unit based on a non-fluorine-containing monomer in addition to the fluorine-containing monomer.
- a non-fluorine-containing monomer olefins having 2 to 4 carbon atoms such as ethylene, propylene and isobutene; vinyl chloride, vinylidene chloride, vinyl acetate, vinyl chloroacetate, vinyl lactate, vinyl butyrate, vinyl pivalate, benzoic acid Vinyl esters such as vinyl acid, vinyl crotonate, methyl (meth) acrylate, ethyl (meth) acrylate, n-butyl (meth) acrylate, methyl crotonate, etc .; methyl vinyl ether (MVE), ethyl vinyl ether (EVE), Vinyl ethers such as butyl vinyl ether (BVE), isobutyl vinyl ether (IBVE), cyclohexyl vinyl ether (CH
- VDF copolymer (C1) composed of at least vinylidene fluoride units (VDF units), for example, vinylidene fluoride homopolymer (polyvinylidene fluoride (polyvinylidene fluoride ( PVDF)) (C1-1), A copolymer comprising a VDF unit and a TFE unit, wherein the content of the VDF unit is 30% by mole or more and 99% by mole or less, based on the entire monomer excluding the functional group-containing monomer described later, and TFE Copolymer (C1-2) in which the content of units is from 1 to 70 mol%, A copolymer comprising VDF units, TFE units, and trichlorofluoroethylene units, wherein the content of VDF units is 10 mol% or more and 90 mol with respect to the entire monomer excluding the functional group-containing monomer described later % Or less, the content of TFE units is
- the content of VDF units is 15 mol% or more and 84 mol% or less, and the content of TFE units with respect to the entire monomers excluding the functional group-containing monomers described later. It is preferable that content of 15 mol% or more and 84 mol% or less and HFP unit is 0 mol% or more and 30 mol% or less.
- the copolymer (C2) comprising at least a tetrafluoroethylene unit (TFE unit) and an ethylene unit (E unit) (hereinafter sometimes referred to as TFE copolymer (C2)), for example, functional groups described later
- TFE copolymer (C2) ethylene unit
- the polymer whose content of a TFE unit is 20 mol% or more with respect to the whole monomer except group-containing monomer is mentioned, Furthermore, the whole monomer except a functional group-containing monomer described later Relative to each other, the content of TFE units is 20 to 80 mol%, the content of E units is 20 to 80 mol%, and the content of units derived from monomers copolymerizable therewith.
- the copolymer etc. whose quantity is 0 mol% or more and 60 mol% or less are mentioned.
- Examples of the copolymerizable monomer include hexafluoropropylene (HFP), the general formula CF 2 FORCFOR f 1 (wherein, R f1 may be an etheric oxygen atom having 1 to 10 carbon atoms).
- HFP hexafluoropropylene
- R f1 may be an etheric oxygen atom having 1 to 10 carbon atoms.
- a fluoroalkyl group the general formula CH 2 CXCX 1 (CF 2 ) n X 2 (wherein, X 1 and X 2 independently represent a hydrogen atom or a fluorine atom, and n is 2 or more and 10 or less) And the like.
- HFP hexafluoropropylene
- CF 2 FORCFOR f 1 wherein, R f1 may be an etheric oxygen atom having 1 to 10 carbon atoms.
- a fluoroalkyl group the general formula CH 2 CXCX 1 (CF 2 ) n X
- TFE copolymer (C2) for example, TFE unit and E unit, and the general formula CH 2 CXCX 1 (CF 2 ) n X 2 (wherein, X 1 and X 2 independently represent a hydrogen atom or a fluorine atom, and n is 2 or more and 10 or less)
- a copolymer comprising fluoroolefin units derived from fluoroolefins, which is an integer), wherein the content of TFE units is relative to the entire monomer excluding the functional group-containing monomer described later.
- the content of E units is 20 mol% or more and 55 mol% or less
- the general formula CH 2 CX 3 (CF 2 ) n X 4 (here, X 3 and X 4 are And n represents an integer of 2 to 10, and the content of the fluoroolefin unit derived from the fluoroolefin is 0 mol% to 10 mol% independently.
- Polymer ( 2-1) A copolymer comprising a TFE unit, an E unit, an HFP unit, and a unit derived from a monomer copolymerizable therewith, wherein the entire monomer excluding the functional group-containing monomer described later,
- the content of TFE unit is 30 mol% or more and 70 mol% or less
- the content of E unit is 20 mol% or more and 55 mol% or less
- the content of HFP unit is 1 mol% or more and 30 mol% or less
- copolymerization with these A copolymer (C2-2) in which the content of units derived from possible monomers is 0 mol% or more and 10 mol% or less, TFE units and E units, and the (in this case, R f1 represents.
- At least a tetrafluoroethylene unit (TFE unit) and a hexafluoropropylene unit (HFP unit) and / or the general formula CF 2 CFOR f 1 (wherein R f1 is an etheric oxygen atom having 1 to 10 carbon atoms)
- a copolymer (C3) (Hereinafter, it may be called a TFE copolymer (C3).) Which consists of a PAVE unit derived from PAVE represented with the perfluoroalkyl group which may be included.
- CTFE units chlorotrifluoroethylene units
- E units ethylene units
- fluorine-containing monomer units It is a chloro trifluoro ethylene copolymer (C4) (Hereinafter, it may be called a CTFE copolymer (C4).).
- the CTFE copolymer (C4) is not particularly limited, and, for example, CTFE / PAVE copolymer, CTFE / VDF copolymer, CTFE / HFP copolymer, CTFE / E copolymer, CTFE / PAVE / E co-polymer Polymers, CTFE / VDF / E copolymers, CTFE / HFP / E copolymers, etc. may be mentioned.
- the content of the CTFE unit in the CTFE copolymer (C4) is preferably 15 mol% or more and 70 mol% or less with respect to the whole monomer excluding the functional group-containing monomer described later, and is 18 mol% It is more preferable that it is 65 mol% or less.
- the content of the E unit and / or the fluorine-containing monomer unit is preferably 30 mol% or more and 85 mol% or less, and more preferably 35 mol% or more and 82 mol% or less.
- the copolymer (C5) comprising at least a chlorotrifluoroethylene unit (CTFE unit) and a tetrafluoroethylene unit (TFE unit) is a CTFE unit [—CFCl—CF 2 —] and a TFE unit [—CF 2 —CF 2] -], And a chlorotrifluoroethylene copolymer composed of monomer units copolymerizable with CTFE and TFE (hereinafter sometimes referred to as CTFE / TFE copolymer (C5)).
- CTFE unit chlorotrifluoroethylene unit
- TFE unit tetrafluoroethylene unit
- R f1 represents a perfluoroalkyl group which may contain an etheric oxygen atom having 1 to 10 carbon atoms.
- R f1 represents a perfluoroalkyl group which may contain an etheric oxygen atom having 1 to 10 carbon atoms.
- R f1 represents a perfluoroalkyl group which may contain an etheric oxygen atom having 1 to 10 carbon atoms.
- R f1 represents a perfluoroalkyl group which may contain an etheric oxygen atom having 1 to 10 carbon atoms.
- PMVE perfluoro (methyl vinyl ether)
- PPVE perfluoro (propyl vinyl ether)
- the CTFE / TFE copolymer (C5) is not particularly limited.
- the total content of CTFE units and TFE units in the CTFE / TFE copolymer (C5) is described later from the viewpoint of securing good formability, environmental stress crack resistance, chemical solution barrier properties, heat resistance, and mechanical properties. It is preferable that it is 90.0 mol% or more and 99.9 mol% or less with respect to the whole monomer except the functional group containing monomer of, and containing of the said CTFE and the monomer unit copolymerizable with TFE.
- the amount is preferably 0.10% by mole or more and 10.0% by mole or less.
- the content of CTFE units in the CTFE / TFE copolymer (C5) is a total amount of CTFE units and TFE units of 100 from the viewpoint of securing good formability, environmental stress crack resistance, and chemical solution barrier properties.
- the content is preferably 15 to 80 mol%, more preferably 17 to 70 mol%, and still more preferably 19 to 65 mol% with respect to the mol%.
- the content of PAVE units is the entire monomer excluding the functional group-containing monomer described later It is preferable that it is 0.5 mol% or more and 7 mol% or less, and it is more preferable that it is 1 mol% or more and 5 mol% or less.
- the total content of HFP units and PAVE units is the functional group-containing monomer described later It is preferable that it is 0.5 to 7 mol% with respect to the whole monomer except these, and it is more preferable that it is 1 to 5 mol%.
- the TFE copolymer (C3), the CTFE copolymer (C4), and the CTFE / TFE copolymer (C5) are excellent in chemical solution barrier properties, particularly barrier properties to alcohol-containing gasoline.
- the permeation coefficient of alcohol-containing gasoline is determined by placing a sheet obtained from the resin to be measured in a cup for measuring the permeability coefficient into which isooctane / toluene / ethanol mixed solvent in which isooctane, toluene and ethanol are mixed at a volume ratio of 45:45:10 , And a value calculated from the mass change measured at 60.degree.
- the alcohol-containing gasoline permeation coefficient of TFE copolymer (C3), CTFE copolymer (C4) and CTFE / TFE copolymer (C5) is 1.5 g ⁇ mm / (m 2 ⁇ day) or less preferably, 0.010g ⁇ mm / (m 2 ⁇ day) or more 1.0 g ⁇ mm / more preferably (m 2 ⁇ day) or less, 0.020g ⁇ mm / (m 2 ⁇ day) or more 0 More preferably, it is not more than .80 g ⁇ mm / (m 2 ⁇ day).
- the fluorine-containing polymer (C) can be obtained by (co) polymerizing monomers constituting the polymer by a conventional polymerization method.
- the method by radical polymerization is mainly used. That is, the means for initiating the polymerization is not limited as long as it progresses radically, but it may be initiated by, for example, an organic or inorganic radical polymerization initiator, heat, light or ionizing radiation.
- the manufacturing method of a fluorine-containing polymer (C) does not have a restriction
- the polymerization method using the radical polymerization initiator generally used is used.
- a polymerization method bulk polymerization, solution polymerization using an organic solvent such as fluorohydrocarbon, chlorohydrocarbon, fluorochlorohydrocarbon, alcohol, hydrocarbon and the like, an aqueous medium and, if necessary, an appropriate organic solvent are used.
- Known methods such as suspension polymerization, emulsion polymerization using an aqueous medium and an emulsifying agent can be adopted.
- the polymerization can be carried out as a batch system or a continuous system using a single tank or multiple tank stirring type polymerization apparatus or a tubular type polymerization apparatus.
- the decomposition temperature at which the half life is 10 hours is preferably 0 ° C. or more and 100 ° C. or less, and more preferably 20 ° C. or more and 90 ° C. or less.
- Specific examples thereof include 2,2′-azobisisobutyronitrile, 2,2′-azobis (2,4-dimethylvaleronitrile), 2,2′-azobis (2-methylvaleronitrile), 2,2 '-Azobis (2-cyclopropylpropionitrile), dimethyl 2,2'-azobisisobutyrate, 2,2'-azobis [2- (hydroxymethyl) propionitrile], 4,4'-azobis (4-cyano Azo compounds such as pentenoic acid); hydroperoxides such as hydrogen peroxide, t-butyl hydroperoxide, cumene hydroperoxide; dialkyl peroxides such as di-t-butyl peroxide, dicumyl peroxide; acetyl peroxide
- a chain transfer agent for molecular weight control.
- alcohols such as methanol and ethanol, 1,3-dichloro-1,1,2,2,3-pentafluoropropane, 1,1-dichloro-1-fluoroethane, 1,2-dichloro- Chlorofluorohydrocarbons such as 1,1,2,2-tetrafluoroethane, 1,1-dichloro-1-fluoroethane, 1,1,2-trichloro-1,2,2-trifluoroethane; pentane, hexane And hydrocarbons such as cyclohexane; and chlorohydrocarbons such as carbon tetrachloride, chloroform, methylene chloride and methyl chloride. One or more of these may be used.
- the polymerization conditions are not particularly limited, and the polymerization temperature is preferably 0 ° C. or more and 100 ° C. or less, and more preferably 20 ° C. or more and 90 ° C. or less. In order to avoid the decrease in heat resistance due to ethylene-ethylene chain formation in the polymer, low temperature is generally preferred.
- the polymerization pressure is appropriately determined in accordance with other polymerization conditions such as the type and amount of the solvent used, the vapor pressure, the polymerization temperature and the like, but is preferably 0.1 MPa or more and 10 MPa or less and is 0.5 MPa or more Is more preferred.
- the polymerization time is preferably 1 hour or more and 30 hours or less.
- the molecular weight of the fluorine-containing polymer (C) is not particularly limited, but it is preferably a polymer which is solid at room temperature and which can be used as a thermoplastic resin, an elastomer or the like.
- the molecular weight is controlled by the concentration of monomers used for polymerization, the concentration of a polymerization initiator, the concentration of a chain transfer agent, and the temperature.
- the melt flow rate at a temperature 50 ° C. higher than the melting point of the fluorine-containing polymer (C) and at a load of 5 kg is 0.5 g / 10 min or more and 200 g / 10 min or less Is preferably, and more preferably 1 g / 10 minutes to 100 g / 10 minutes.
- the melting point and the glass transition temperature of the polymer can be adjusted by selecting the kind of fluorine-containing monomer and other monomers, the composition ratio, and the like of the fluorine-containing polymer (C).
- the melting point of the fluorine-containing polymer (C) is appropriately selected depending on the purpose, use, and method of use, but in the case of coextrusion with the aliphatic polyamide composition (A) and the semiaromatic polyamide composition (B) etc. And preferably close to the molding temperature of the resin. Therefore, it is preferable to optimize the melting point of the fluorine-containing polymer (C) by appropriately adjusting the proportions of the fluorine-containing monomer and other monomers and the functional group-containing monomer described later.
- the melting point refers to heating the sample to a temperature above the expected melting point using a differential scanning calorimeter, and then cooling the sample to a temperature of 10 ° C. per minute and cooling to 30 ° C.
- the temperature at the peak value of the melting curve which is measured by leaving it for about 1 minute and then raising the temperature at a rate of 10 ° C. per minute, is defined as the melting point.
- the fluorine-containing polymer (C) has a functional group having reactivity with amino groups in the molecular structure, and the functional group is the molecular terminal, side chain or side of the fluorine-containing polymer (C). It may be contained in any of the main chains.
- the functional group may be used singly or in combination of two or more types in the fluorine-containing polymer (C).
- the type and content of the functional group are appropriately determined according to the type, shape, application, required interlayer adhesion, adhesion method, functional group introduction method and the like of the counterpart material to be laminated on the fluorine-containing polymer (C) Ru.
- the functional group having reactivity with amino group is selected from the group consisting of carboxyl group, acid anhydride group or carboxylate, sulfo group or sulfonate, epoxy group, cyano group, carbonate group, and haloformyl group
- the fluorine-containing polymer (C) manufactured from said (i) and (ii) is preferable.
- JP-A-173447 and JP-A-10-503236 please refer to the manufacturing method according to JP-A-173447 and JP-A-10-503236.
- a polymerized monomer comprising at least one functional group-containing monomer selected from the group consisting of a carboxyl group, an acid anhydride group or carboxylate, a hydroxyl group, a sulfo group or sulfonate, an epoxy group, and a cyano group Use.
- a functional group containing monomer a functional group containing non-fluorine monomer, a functional group containing fluorine-containing monomer, etc. are mentioned.
- acrylic acid halogenated acrylic acid (with the exception of fluorine), methacrylic acid, halogenated methacrylic acid (with the exception of fluorine), maleic acid, halogenated maleic acid (with the exception of (Excluding fluorine), fumaric acid, halogenated fumaric acid (excluding fluorine), itaconic acid, citraconic acid, crotonic acid, endobicyclo- [2.2.1] -5-heptene-2,3-dicarboxylic acid Unsaturated carboxylic acids such as acids and derivatives thereof; maleic anhydride, itaconic anhydride, succinic anhydride, citraconic anhydride, endobicyclo- [2.2.1] -5-heptene-2,3-dicarboxylic acid Carboxyl group-containing monomer such as anhydride; Epoxy group-containing monomer such as glycidyl acrylate, glycidyl me
- The. One or more of these may be used.
- the functional group-containing non-fluorine monomer is determined in consideration of the copolymerization reactivity with the fluorine-containing monomer to be used. By selecting a suitable functional group-containing non-fluorine monomer, the polymerization proceeds well, and it is easy to introduce uniformly into the main chain of the functional group-containing non-fluorine monomer, resulting in less unreacted monomer There is an advantage that impurities can be reduced.
- An unsaturated compound represented by As the carboxyl group-derived group which is Y in the above general formula, for example, general formula -C ( O) Q 1 (wherein, Q 1 is -OR 8 , -NH 2 , F, Cl, Br or I) R 8 represents an alkyl group having 1 or more and 20 or less carbon atoms or an aryl group having 6 or more and 22 or less carbon atoms.
- a sulfonic acid-derived group which is Y in the above general formula for example, a general formula -SO 2 Q 2 (wherein, Q 2 represents -OR 9 , -NH 2 , F, Cl, Br or I, and R 9 And the group represented by the alkyl group of 1 or more and 20 or less carbon atoms or the aryl group of 6 or more and 22 or less carbon atoms.
- the Y is preferably -COOH, -SO 3 H, -SO 3 Na, -SO 2 F or -CN.
- the functional group-containing fluorine-containing monomer for example, when it is a functional group having a carbonyl group, perfluoroacrylic acid fluoride, 1-fluoroacrylic acid fluoride, acrylic acid fluoride, 1-trifluoromethacrylic acid fluoride, perfluoro Butene acid etc. are mentioned. One or more of these may be used.
- the content of the functional group-containing monomer in the fluorine-containing polymer (C) secures sufficient interlayer adhesion, does not cause deterioration in interlayer adhesion depending on the use environment conditions, and secures sufficient heat resistance From the viewpoint of preventing the occurrence of peeling, coloring, foaming, elution, etc. due to decomposition at the time of processing at high temperature, adhesion failure, coloring, foaming, use at high temperature, etc. % Or more and 5.0 mol% or less, preferably 0.015 mol% or more and 4.0 mol% or less, and more preferably 0.02 mol% or more and 3.0 mol% or less preferable.
- the polymerization rate at the time of production does not decrease, and the fluorine-containing polymer (C) is excellent in the adhesiveness to the partner material to be laminated.
- the method of adding the functional group-containing monomer is not particularly limited, and may be added all at once at the start of the polymerization, or may be added continuously during the polymerization. The method of addition is appropriately selected depending on the decomposition reactivity of the polymerization initiator and the polymerization temperature, but during the polymerization, the consumed amount is continuously or intermittently consumed as the functional group-containing monomer is consumed in the polymerization.
- the polymerization tank It is preferable to supply in the polymerization tank and maintain the concentration of the functional group-containing monomer in this range.
- content of the functional group containing monomer in a fluorine-containing copolymer (C) 0.01 mol% with respect to all the polymerization units is the function in a fluorine-containing copolymer (C)
- the content of the group residue corresponds to 100 per 1 ⁇ 10 6 carbon atoms in the main chain of the fluorine-containing copolymer (C).
- 5.0 mol% of the content of the functional group residue in the fluorine-containing copolymer (C) is a fluorine-containing copolymer with 5.0 mol% with respect to all the polymerization units in the fluorine-containing copolymer (C) This corresponds to 50,000 for the main chain carbon number of 1 ⁇ 10 6 in (C).
- a mixture of a fluorine-containing polymer in which a functional group is introduced and a fluorine-containing polymer in which a functional group is not introduced may be used.
- the functional group is introduced to one or both ends of the molecular chain of the fluorine-containing polymer.
- a functional group introduced at the end a carbonate group and a haloformyl group are preferable.
- R 10 is a hydrogen atom, an organic group (for example, an alkyl group having 1 to 20 carbon atoms, an alkyl group having 2 to 20 carbon atoms having an ether bond, etc.), or a group I, II or VII element .
- the haloformyl group is specifically -COZ [Z is a halogen element. ], And includes -COF, -COCl, and the like. One or more of these may be used.
- a carbonate group at the molecular terminal of the polymer various methods using a polymerization initiator and / or a chain transfer agent can be adopted, but peroxides, particularly peroxycarbonates and / or peroxyesters.
- the method of using as a polymerization initiator can be preferably adopted from the viewpoint of performance such as economy, heat resistance, and chemical resistance.
- a carbonyl group derived from peroxide for example, a carbonate group derived from peroxycarbonate, an ester group derived from peroxyester, or a haloformyl group polymer formed by converting these functional groups It can be introduced at the end.
- these polymerization initiators it is more preferable to use peroxy carbonate because the polymerization temperature can be lowered and the initiation reaction does not involve a side reaction.
- the carbonate group of the fluorine-containing polymer having the above-mentioned carbonate group at the end is heated to thermally decompose (decarboxylation) It can be obtained by
- peroxy carbonate diisopropyl peroxy carbonate, di-n-propyl peroxy carbonate, t-butyl peroxy isopropyl carbonate, t-butyl peroxy methacryloyloxyethyl carbonate, bis (4-t-butylcyclohexyl) peroxy Dicarbonate, di-2-ethylhexyl peroxydicarbonate and the like can be mentioned. One or more of these may be used.
- the amount of peroxycarbonate used varies depending on the type (composition etc.) of the target polymer, molecular weight, polymerization conditions, and type of initiator used, but the polymerization rate is appropriately controlled to ensure a sufficient polymerization rate
- 100 parts by mass of the total polymer obtained by polymerization is preferably 0.05 parts by mass or more and 20 parts by mass or less, and more preferably 0.1 parts by mass or more and 10 parts by mass or less.
- the carbonate group content at the molecular terminal of the polymer can be controlled by adjusting the polymerization conditions.
- the addition method of the polymerization initiator is not particularly limited, and may be added all at once at the start of the polymerization or continuously during the polymerization. The method of addition is appropriately selected depending on the decomposition reactivity of the polymerization initiator and the polymerization temperature.
- the terminal functional group number with respect to the main chain carbon number of 10 6 in the fluorine-containing polymer (C) secures sufficient interlayer adhesion, does not cause deterioration in interlayer adhesion depending on the use environment conditions, and is heat resistant.
- 150 or more and 3,000 or less from the viewpoint of sufficiently securing and preventing the occurrence of peeling, coloring, foaming, elution, etc. due to decomposition at the time of processing at high temperature, adhesion failure, coloring, foaming, use at high temperature Is preferably 200 to 2,000, and more preferably 300 to 1,000.
- a mixture of a fluorine-containing polymer in which a functional group is introduced and a fluorine-containing polymer in which a functional group is not introduced may be used.
- the fluorine-containing polymer (C) is a fluorine-containing polymer in which a functional group having reactivity to an amino group is introduced.
- the fluorine-containing polymer (C) into which a functional group has been introduced is itself heat resistance, water resistance, low friction, chemical resistance, weather resistance, stain resistance unique to fluorine-containing polymers It is possible to maintain excellent properties such as chemical liquid barrier properties, which is advantageous in terms of productivity and cost.
- the fluorine-containing polymer (C) can be added with various fillers such as inorganic powder, glass fiber, carbon fiber, metal oxide or carbon within a range not to impair the performance depending on the purpose and application.
- various fillers such as inorganic powder, glass fiber, carbon fiber, metal oxide or carbon within a range not to impair the performance depending on the purpose and application.
- pigments, UV absorbers and other optional additives may be mixed.
- other fluororesins, resins such as thermoplastic resins, and synthetic rubbers can also be added to improve mechanical properties, improve weatherability, impart design properties, prevent static, and form It is possible to improve the quality etc.
- the first embodiment of the laminated tube includes at least two layers of (a) layer and (b) layer, and at least one set of (a) layer and (b) layer are disposed adjacent to each other.
- the laminated tube of the first embodiment it is essential to include the (b) layer, and the chemical solution barrier property, particularly the hydrocarbon barrier property, of the laminated tube becomes good. Furthermore, by arranging the (a) layer and the (b) layer adjacent to each other, it is possible to obtain a laminated tube excellent in interlayer adhesion and its durability.
- the (b) layer is disposed inside the (a) layer.
- the (a) layer is disposed on the outermost layer of the laminated tube.
- the (b) layer is disposed in the innermost layer of the laminated tube.
- (B) By arranging the layer in the innermost layer, it is possible to obtain a laminated tube excellent in deterioration fuel resistance, and to suppress the elution of low molecular weight components such as monomers and oligomers due to contact with alcohol-containing gasoline. Become. That is, it is more preferable to use a laminated tube in which the (a) layer is disposed in the outermost layer and the (b) layer is disposed in the innermost layer.
- the conductive layer containing the semiaromatic polyamide composition (B) containing the conductive filler when used as a fuel piping tube, it prevents sparks generated by the internal friction of the fuel circulating in the piping or the friction with the tube wall from igniting the fuel It is possible to At that time, it is possible to achieve both low-temperature impact resistance and conductivity by placing a layer containing a semi-aromatic polyamide having no conductivity on the outside with respect to the conductive layer, and economy Is also advantageous.
- Conductivity means that, for example, when a flammable fluid such as gasoline comes into contact with an insulator such as a resin continuously, static electricity may accumulate and ignite, but this static electricity does not accumulate. It is said to have electrical characteristics. This makes it possible to prevent explosion due to static electricity that is generated when transporting a fluid such as fuel.
- the conductive filler includes all fillers added for imparting conductive performance to the resin, and includes particulate, flake, and fibrous fillers.
- Examples of the particulate filler include carbon black and graphite.
- Examples of the flake filler include aluminum flakes, nickel flakes, nickel-coated mica and the like.
- Examples of fibrous fillers include metal fibers such as carbon fibers, carbon-coated ceramic fibers, carbon whiskers, carbon nanotubes, aluminum fibers, copper fibers, brass fibers, stainless steel fibers and the like. One or more of these may be used. Among these, carbon nanotubes and carbon black are preferable.
- Carbon nanotubes are referred to as hollow carbon fibrils, which have an outer region consisting of an essentially continuous multiple layer of regularly arranged carbon atoms and an inner hollow region, each layer being And the hollow region are essentially cylindrical fibrils arranged substantially concentrically around the cylindrical axis of the fibrils. Furthermore, it is preferable that the regularly arranged carbon atoms of the outer region be graphitic, and the diameter of the hollow region be 2 nm or more and 20 nm or less.
- the outer diameter of the carbon nanotube is preferably 3.5 nm or more and 70 nm or less, and is 4 nm or more and 60 nm or less, from the viewpoint of providing sufficient dispersibility in the resin and good conductivity of the obtained resin molded body. Is more preferred.
- the aspect ratio (a ratio of length / outer diameter) of the carbon nanotube is preferably 5 or more, more preferably 100 or more, and still more preferably 500 or more. By satisfying the aspect ratio, a conductive network can be easily formed, and excellent conductivity can be exhibited with a small amount of addition.
- Carbon black includes all carbon blacks generally used for imparting conductivity, and preferred carbon blacks include acetylene black obtained by incomplete combustion of acetylene gas and furnace-type incomplete combustion from crude oil Furnace black such as ketjen black, oil black, naphthalene black, thermal black, lamp black, channel black, roll black, disc black, etc., but not limited thereto. Among these, acetylene black and furnace black are more preferable.
- various carbon powders having different properties such as particle diameter, surface area, DBP oil absorption, and ash content have been manufactured.
- the characteristics of the carbon black are not limited, but those having a good chain structure and a large cohesive density are preferable.
- a large amount of carbon black is not preferable from the viewpoint of impact resistance, and from the viewpoint of obtaining excellent electric conductivity in a smaller amount, the average particle diameter is preferably 500 nm or less, more preferably 5 nm or more and 100 nm or less
- the surface area (BET method) is preferably 10 m 2 / g or more, more preferably 30 m 2 / g or more, and 50 m 2 / g or more.
- the DBP (dibutyl phthalate) oil absorption is preferably 50 ml / 100 g or more, more preferably 100 ml / 100 g, and still more preferably 150 ml / 100 g or more.
- the ash content is preferably 0.5% by mass or less, and more preferably 0.3% by mass or less.
- the DBP oil absorption is a value measured by the method defined in ASTM D-2414.
- the volatile content of carbon black is preferably less than 1% by mass.
- These conductive fillers may be subjected to surface treatment with a surface treatment agent such as titanate, aluminum or silane. It is also possible to use granulated ones to improve melt-kneading workability.
- the content of the conductive filler varies depending on the type of the conductive filler to be used, and thus can not be generally specified, but from the viewpoint of balance with conductivity, fluidity, mechanical strength, etc., semiaromatic polyamide (B1) or It is preferable that it is generally 3 mass parts or more and 30 mass parts or less with respect to 100 mass parts of semi-aromatic polyamide (B2). Further, from the viewpoint of obtaining sufficient antistatic performance, the conductive filler preferably has a surface specific resistance value of 10 8 ⁇ / square or less, more preferably 10 6 ⁇ / square or less. preferable. However, the addition of the conductive filler tends to deteriorate the strength and the flowability. Therefore, it is desirable that the content of the conductive filler be as small as possible if the target conductivity level is obtained.
- the thickness of each layer is not particularly limited, and may be adjusted according to the type of polymer constituting each layer, the total number of layers in the laminated tube, the application, etc. , It is determined in consideration of the properties such as chemical solution barrier property, low temperature impact resistance, and flexibility of the laminated tube.
- the thickness of each of the layers (a) and (b) is preferably 3% or more and 90% or less with respect to the total thickness of the laminated tube.
- the thickness of the layer (b) is more preferably 5% or more and 50% or less, more preferably 7% or more and 30% or less, based on the total thickness of the laminated tube, in consideration of the balance between low temperature impact resistance and chemical liquid barrier property. It is more preferable that it is the following.
- the total number of layers in the laminated tube of the first aspect is not particularly limited as long as it is at least two layers including the (a) layer and the (b) layer.
- the laminated tube according to the first aspect has another thermoplastic resin in order to impart a further function or to obtain an economically advantageous laminated tube.
- the layer to be contained may have one or more layers.
- the number of layers of the laminated tube of the first embodiment is two or more, but it is preferably eight or less as judged from the mechanism of the tube manufacturing apparatus, and more preferably two or more and seven or less.
- the second aspect of the laminated tube further includes at least three layers having (c) layers in the first aspect, and at least one set of (b) layers and (c) layers are disposed adjacent to each other.
- the laminated tube of the second aspect it is essential to include the (b) layer, and the chemical solution barrier property, particularly the hydrocarbon barrier property, of the laminated tube becomes good. It is also essential to include the (c) layer, and the chemical solution barrier properties of the laminated tube, in particular, the alcohol barrier properties and the barrier properties to the high concentration alcohol-containing gasoline become good. Furthermore, by arranging the (b) layer and the (c) layer adjacent to each other, it is possible to obtain a laminated tube excellent in interlayer adhesion and its durability.
- the (c) layer is disposed inside the (b) layer.
- the (b) layer is disposed between the (a) layer and the (c) layer.
- the (a) layer is disposed on the outermost layer of the laminated tube. (A) By arranging the layers in the outermost layer, it is possible to obtain a laminated tube excellent in chemical resistance and flexibility. Also, the (b) layer is disposed between the (a) layer and the (c) layer.
- a laminated tube having excellent deterioration fuel resistance can be obtained, and elution of low molecular weight components such as monomers and oligomers by contact with alcohol-containing gasoline Can be suppressed. That is, a laminated tube in which (a) layer is disposed in the outermost layer, (b) layer is disposed in the middle layer, and (c) layer is disposed in the innermost layer is preferable.
- the conductive layer containing the fluorine-containing polymer composition containing the conductive filler when used as a fuel piping tube, chemical solution barrier property, deterioration fuel resistance, And excellent in the elution resistance of monomers and oligomers, and when used as a fuel piping tube, to prevent sparks generated by the internal friction of the fuel circulating in the piping or friction with the tube wall from igniting the fuel Is possible.
- the fluorine-containing polymer mentioned here also includes the fluorine-containing polymer (C) having a functional group in the molecular chain, and also refers to a fluorine-containing polymer having no functional group described later.
- the details of the conductive and conductive fillers are the same as in the laminated tube of the first embodiment.
- the content of the conductive filler varies depending on the type of the conductive filler to be used, and thus can not be generally specified, but from the viewpoint of balance with conductivity, fluidity, mechanical strength, etc., 100 parts by mass of fluorine-containing polymer In general, it is preferably 3 parts by mass or more and 30 parts by mass or less. Further, from the viewpoint of obtaining sufficient antistatic performance, the conductive filler preferably has a surface specific resistance value of 10 8 ⁇ / square or less, more preferably 10 6 ⁇ / square or less. preferable. However, the addition of the conductive filler tends to deteriorate the strength and the flowability. Therefore, it is desirable that the content of the conductive filler be as small as possible if the target conductivity level is obtained.
- the thickness of each layer is not particularly limited, and may be adjusted according to the type of polymer constituting each layer, the number of all layers in the laminated tube, the application, etc. , It is determined in consideration of the properties such as chemical solution barrier property, low temperature impact resistance, and flexibility of the laminated tube.
- the thickness of each of the (a) layer, the (b) layer, and the (c) layer is preferably 3% or more and 90% or less with respect to the total thickness of the laminated tube. It is more preferable that the thicknesses of the (b) layer and the (c) layer be 5% or more and 50% or less with respect to the total thickness of the laminated tube in consideration of the balance between low temperature impact resistance and chemical liquid barrier property. More preferably, it is 7% or more and 30% or less.
- the total number of layers in the laminated tube of the second aspect is not particularly limited as long as it is at least three layers including (a) layer, (b) layer, and (c) layer.
- the laminated tube of the second aspect has a further function in addition to the three layers of (a), (b), and (c) layers, or in order to obtain an economically advantageous laminated tube, It may have one or more layers containing other thermoplastic resins.
- the number of layers of the laminated tube of the second embodiment is three or more, but it is preferably eight or less as judged from the mechanism of the tube manufacturing apparatus, and more preferably three or more and seven or less.
- PVDF polyvinylidene fluoride
- PVF polyvinyl fluoride
- PTFE polytetrafluoroethylene
- PCTFE polychlorotrifluoroethylene
- FEP Tetrafluoroethylene / hexafluoropropylene copolymer
- EEP Tetrafluoroethylene / hexafluoropropylene copolymer
- EEP Tetrafluoroethylene / perfluoro (alkyl vinyl ether) / hexafluoropropylene copolymer
- ETFE ethylene / tetrafluoroethylene copolymer
- EEP ethylene / tetrafluoroethylene / Hexafluoropropylene copolymer
- EEP vinylidene fluoride / tetrafluoroethylene copolymer
- vinylidene fluoride / tetrafluoroethylene copolymer vinylidene fluoride / hexaflu
- the layer containing the fluorine-based polymer having no functional group is disposed on the inner side with respect to the (c) layer, so that the low temperature impact resistance, the chemical solution barrier property, And environmental stress crack resistance can be compatible, and it is also economically advantageous.
- high density polyethylene high density polyethylene
- MDPE medium density polyethylene
- LDPE low density polyethylene
- LLDPE linear low density polyethylene
- UHMWPE ultra high molecular weight polyethylene
- PP polypropylene
- PB polybutene
- TPX Polymethylpentene
- EPR ethylene / propylene copolymer
- EBR ethylene / butene copolymer
- EAA ethylene / vinyl acetate copolymer
- EAA acrylic acid copolymer
- Polyolefins such as ethylene / methacrylic acid copolymer (EMAA), ethylene / methyl acrylate copolymer (EMA), ethylene / methyl methacrylate copolymer (EMMA), ethylene / ethyl acrylate copolymer (EEA) Resin; polystyrene (PS), syndiotactic polymer Styrene (SPS), methyl methacrylate / styren
- Cellulose based resins Cellulose based resins; Polycarbonate based resins such as polycarbonate (PC); Thermoplastic polyimides (TPI), Polyether imides, polyester imides, polyester imides, polyamide imides (PAI), Polyimides based resins such as polyester amide imide; Thermoplastic polyurethane based resins; Polyamide elastomers, polyurethane elastomers, polyester elastomers and the like can be mentioned.
- PC polycarbonate
- TPI Thermoplastic polyimides
- PAI polyamide imides
- Polyimides based resins such as polyester amide imide
- Thermoplastic polyurethane based resins Polyamide elastomers, polyurethane elastomers, polyester elastomers and the like can be mentioned.
- polyester resins having a melting point of 290 ° C. or less among the thermoplastic resins exemplified above, polyester resins having a melting point of 290 ° C. or less, polyamide resins, polythioether resins, from the viewpoint of melting stability and molding stability, It is preferable to use a polyolefin-based resin and a fluorine-based polymer not containing a functional group.
- polyester resins having a melting point of 290 ° C. or less, polyamide resins, polythioether resins among the thermoplastic resins exemplified above. It is preferable to use a polyolefin-based resin and a fluorine-based polymer not containing a functional group.
- any base material other than thermoplastic resin for example, paper, metal-based material, non-oriented, uniaxially or biaxially stretched plastic film or sheet, woven fabric, non-woven fabric, metallic cotton, wood, etc.
- metal-based materials metals such as aluminum, iron, copper, nickel, gold, silver, titanium, molybdenum, magnesium, manganese, lead, tin, chromium, beryllium, tungsten, cobalt, metal compounds, and two or more of these Alloys such as stainless steel, aluminum alloys, brass, copper alloys such as bronze, alloys such as nickel alloys, and the like.
- a laminated tube manufacturing method melt extrusion, a method of simultaneously laminating in or out of a die (coextrusion molding method) using an extruder corresponding to the number of layers or the number of materials, or a single layer tube or A method (coating method) is available in which the laminated tube manufactured by the above method is manufactured in advance, and an adhesive is used on the outside sequentially as needed to integrate the resin.
- the laminated tube is preferably manufactured by a co-extrusion method in which various materials are co-extruded in a molten state and heat fusion (fusion bonding) of the two is performed to produce a tube having a laminated structure in one step. That is, it is preferable that the method for producing a laminated tube includes co-extrusion.
- the above-mentioned laminated tube is formed to remove the residual strain of the molded product, It is also possible to obtain a target molded article by heat treatment at a temperature less than the lowest melting point of the melting points of the resin constituting the tube for 0.01 hours or more and 10 hours or less.
- the laminated tube may have a corrugated area.
- the waveform area is an area formed in a waveform shape, a bellows shape, an accordion shape, a corrugated shape or the like.
- the corrugated area may not only be provided over the entire length of the laminated tube but may be partially provided in an appropriate area on the way.
- the corrugated area can be easily formed by first molding a straight tubular tube and subsequently molding it to form a predetermined corrugated shape or the like. By having such a corrugated area, it is possible to have shock absorption and to facilitate attachment. Furthermore, for example, it is possible to make the shape of an L character, a U character, etc. by adding required parts, such as a connector, or bending.
- natural rubber NR
- BR butadiene rubber
- IR isoprene rubber
- the protective member may be a sponge-like porous body by a known method. By using a porous body, it is possible to form a protective portion that is lightweight and excellent in heat insulation. Also, the material cost can be reduced. Alternatively, glass fiber or the like may be added to improve the strength.
- the shape of the protective member is not particularly limited, it is usually a block-like member having a recess for receiving a tubular member or a laminated tube. In the case of a tubular member, the laminated tube can be inserted later into a tubular member prepared in advance, or the tubular member can be coated and extruded on the laminated tube so that they are in close contact with each other.
- an adhesive is applied to the inner surface of the protective member or the concave as necessary, the laminated tube is inserted or fitted into this, and the two are adhered to integrate the laminated tube and the protective member. Form a structure. Moreover, it is also possible to reinforce with metal etc.
- the outer diameter of the laminated tube takes into consideration the flow rate of the chemical solution (for example, fuel such as alcohol-containing gasoline), the thickness does not increase the permeability of the chemical solution, and the thickness is such that the normal tube breaking pressure can be maintained. And, the tube is easy to assemble and the vibration resistance at the time of use is designed to a thickness that can maintain a good degree of flexibility, but it is not limited. It is preferable that an outer diameter is 4 mm or more and 300 mm or less, an inner diameter is 3 mm or more and 250 mm or less, and a thickness is 0.5 mm or more and 25 mm or less.
- the chemical solution for example, fuel such as alcohol-containing gasoline
- the thickness does not increase the permeability of the chemical solution
- the thickness is such that the normal tube breaking pressure can be maintained.
- the tube is easy to assemble and the vibration resistance at the time of use is designed to a thickness that can maintain a good degree of flexibility, but it is not limited. It is preferable that an outer diameter is 4 mm or more
- the laminated tube of this embodiment includes mechanical parts such as automobile parts, internal combustion engines, electric tool housings, etc., industrial materials, industrial materials, electric and electronic parts, medical care, food, household and office supplies, building materials related parts, It is possible to use for various uses, such as parts for furniture.
- the laminated tube is excellent in chemical solution barrier properties, it is suitable as a chemical solution transfer tube.
- the chemical solution include aromatic hydrocarbon solvents such as benzene, toluene and xylene; alcohols such as methanol, ethanol, propanol, butanol, pentanol, ethylene glycol, propylene glycol, diethylene glycol, phenol, cresol, polyethylene glycol and polypropylene glycol Phenol solvents; ether solvents such as dimethylether, dipropylether, methyl-t-butylether, ethyl-t-butylether, dioxane, tetrahydrofuran etc .; chloroform, methylene chloride, trichloroethylene, ethylene dichloride, perchlorethylene, monochloroethane, dichloroethane, Halogen solvents such as tetrachloroethane, perchlorethane, chlorobenzene; ace
- a laminated tube is suitable as a tube for transporting the chemical solution, and specifically, a feed tube, a return tube, an evaporation tube, a fuel filler tube, an ORVR tube, a reserve tube, a fuel tube such as a reserve tube, a vent tube, an oil tube, petroleum Drilling tube, brake tube, tube for window oscillator fluid, engine coolant (LLC) tube, reservoir tank tube, urea solution transfer tube, cooler tube for coolant water, refrigerant etc. tube for air conditioner refrigerant, heater tube, load heating tube Floor heating tubes, infrastructure supply tubes, tubes for fire extinguishers and fire extinguishing equipment, tubes for medical cooling equipment, inks, paint dispersion tubes, and other chemical solution tubes.
- LLC engine coolant
- the present invention includes the use of the laminated tube as a fuel tube.
- the characteristics of the polyamide resin were measured by the following method. [Relative viscosity] According to JIS K-6920, it was measured under the conditions of a polyamide concentration of 1% and a temperature of 25 ° C. in 96% sulfuric acid.
- Terminal amino group concentration of polyamide (A1), polyamide (A2) Place a predetermined amount of polyamide sample in a stoppered Erlenmeyer flask, add 40 mL of solvent phenol / methanol (volume ratio 9/1) prepared beforehand, dissolve with stirring using a magnetic stirrer, and use thymol blue as an indicator The mixture was titrated with 0.05 N hydrochloric acid to determine the terminal amino group concentration.
- Terminal carboxyl group concentration of polyamide (A1), polyamide (A2) A predetermined amount of polyamide sample is placed in a three-necked pear-shaped flask, 40 mL of benzyl alcohol is added, and the sample is immersed in an oil bath set at 180 ° C. under a nitrogen stream. The mixture was stirred and dissolved by a stirring motor attached to the top, and titration was performed with a 0.05 N sodium hydroxide solution using phenolphthalein as an indicator to determine the terminal carboxyl group concentration.
- Total Concentration of Carboxyl Group and Acid Anhydride Group of Elastomer Polymer (A3) A predetermined amount of elastomer polymer sample is placed in a three-necked pear-shaped flask, dissolved in 170 mL of toluene, and then 30 mL of ethanol is added to prepare a sample solution using phenolphthalein as an indicator, 0.1 N KOH ethanol The solution was titrated to determine the total concentration of carboxyl group and acid anhydride group.
- the properties of the fluorine-containing polymer were measured by the following method. [Composition of fluorine-containing polymer] It was measured by molten NMR analysis, fluorine content analysis, and infrared absorption spectrum.
- each physical property of the laminated tube was measured by the following method.
- [Chemical resistance (zinc chloride resistance)] A polyamide 12 joint was pressed into the end of the tube, and zinc chloride immersion was performed according to the method described in SAE J-2260 7.12. After that, the sample was taken out, and the occurrence of cracks was confirmed. Thereafter, an impact test was carried out at -40.degree. C. according to the method described in SAE J-2260 7.5.
- the tube cut to 200 mm was further cut in half in the longitudinal direction to prepare a test piece.
- a 90 ° peel test was performed using a universal material tester (Tensilon UTM III-200, manufactured by Orientec Co., Ltd.) at a tensile speed of 50 mm / min. The peel strength was read from the maximum point of the SS curve, and the interlayer adhesion was evaluated.
- Polyamide (A1) Production of polyamide 12 (A1-1) In a pressure-resistant reaction vessel with a stirrer having an inner volume of 70 liters, 19.73 kg (100.0 moles) of dodecane lactam, 45. 5-amino-1,3,3-trimethylcyclohexanemethylamine. 0 g (0.264 mol) and 0.5 L of distilled water were charged, and the inside of the polymerization tank was replaced with nitrogen, and then heated to 180 ° C., and stirred at this temperature so that the inside of the reaction system became uniform.
- the temperature in the polymerization tank was raised to 270 ° C., and polymerization was carried out with stirring for 2 hours while regulating the pressure in the tank to 3.5 MPa. Thereafter, the pressure was released to normal pressure over about 2 hours, then the pressure was reduced to 53 kPa, and polymerization was performed for 5 hours under reduced pressure. Next, nitrogen was introduced into the autoclave, and after repressurization to normal pressure, it was extracted as a strand from the lower nozzle of the reaction vessel and cut to obtain a pellet.
- polyamide 12 having a relative viscosity of 2.10, a terminal amino group concentration of 48 ⁇ eq / g, and a terminal carboxyl group concentration of 24 ⁇ eq / g (hereinafter, this polyamide 12 is referred to as (A1-1)).
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups of the polyamide 12 (A1-1) to the number of amide groups is 11.0 and satisfies 8.0 or more.
- the solubility parameter SP value of polyamide 12 (A1-1) is 22.5 (MPa) 1/2 .
- the terminal amino group concentration [A] ( ⁇ eq / g) and the terminal carboxyl group concentration [B] ( ⁇ eq / g) of the polyamide 12 (A1-1) satisfy [A]> [B] +10.
- polyamide 1010 having a relative viscosity of 2.22, a terminal amino group concentration of 45 ⁇ eq / g, and a terminal carboxyl group concentration of 28 ⁇ eq / g (hereinafter, this polyamide 1010 is referred to as (A1-2)).
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups of the polyamide 1010 (A1-2) is 9.0 and satisfies 8.0 or more.
- the solubility parameter SP value of polyamide 1010 (A1-2) is 23.5 (MPa) 1/2 .
- the terminal amino group concentration [A] ( ⁇ eq / g) and the terminal carboxyl group concentration [B] ( ⁇ eq / g) of the polyamide 1010 (A1-2) satisfy [A]> [B] +10.
- a pressure-resistant reaction vessel with a stirrer having an inner volume of 70 liters 9.90 kg (87.5 mol) of caprolactam, 2.69 kg (12.5 mol) of 12-aminododecanoic acid, Add 20.0 g (0.12 mol) of 5-amino-1,3,3-trimethylcyclohexanemethylamine and 2.0 L of distilled water, heat to 100 ° C., and make the reaction system homogeneous at this temperature It stirred so that it might become. Subsequently, the temperature was further raised to 260 ° C. and stirred for 1 hour under a pressure of 2.5 MPa.
- the pressure was released to carry out a polymerization reaction at 260 ° C. for 2 hours under normal pressure while volatilizing water from the reaction vessel, and then a polymerization reaction was performed for 4 hours under a reduced pressure of 260 ° C. and 53 kPa.
- the reaction product taken out in the form of a strand from the lower nozzle of the reaction vessel was introduced into a water bath, cooled, and cut to obtain pellets.
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups of the polyamide 6/12 (A2-1) is 5.75 and is less than 8.0.
- the solubility parameter SP value of polyamide 6/12 (A2-1) is 26.4 (MPa) 1/2 .
- the terminal amino group concentration [A] ( ⁇ eq / g) and the terminal carboxyl group concentration [B] ( ⁇ eq / g) of the polyamide 6/12 (A2-1) satisfy [A]> [B] +10.
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups of the polyamide 6 (A2-2) to the number of amide groups is 5.0 and less than 8.0.
- the solubility parameter SP value of polyamide 6 (A2-2) is 26.9 (MPa) 1/2 .
- the terminal amino group concentration [A] ( ⁇ eq / g) and the terminal carboxyl group concentration [B] ( ⁇ eq / g) of the polyamide 6 (A2-2) satisfy [A]> [B] +10.
- the ratio [CH 2 ] / [NHCO] of the number of methylene groups to the number of amide groups of the polyamide 610 (A2-3) is 7.0 and less than 8.0.
- the solubility parameter SP value of polyamide 610 (A2-3) is 24.9 (MPa) 1/2 .
- the terminal amino group concentration [A] ( ⁇ eq / g) and the terminal carboxyl group concentration [B] ( ⁇ eq / g) of the polyamide 610 (A2-3) satisfy [A]> [B] +10.
- the same polyamide does not correspond to polyamide (A1) because it has an aromatic skeleton as a repeating unit.
- the solubility parameter SP value of polyamide 6T / 6I (A2-4) is 27.8 (MPa) 1/2 .
- the terminal amino group concentration [A] ( ⁇ eq / g) and the terminal carboxyl group concentration [B] ( ⁇ eq / g) of the polyamide 6T / 6I (A2-4) satisfy [A]> [B] +10.
- Elastomer polymer (A3) Maleic anhydride-modified ethylene / 1-butene copolymer (A3-1) (manufactured by Mitsui Chemicals, Inc., Tafmer MH5010, acid anhydride group concentration: 50 ⁇ eq / g)
- Maleic anhydride-modified ethylene / 1-butene copolymer (A3-2) (manufactured by Mitsui Chemicals, Inc., Tafmer MH5020, acid anhydride group concentration: 100 ⁇ eq / g)
- Aliphatic polyamide composition Production of polyamide 12 composition (A-1) Polyamide 12 (A1-1), polyamide 6/12 (A2-1), maleic anhydride-modified ethylene / 1-butene copolymer (A3-1), antioxidant Triethylene glycol-bis [3- (3-t-butyl-5-methyl-4-hydroxyphenyl) propionate] (BASF Japan Ltd., IRGANOX 245), and tris (2,4-di) as a phosphorus-based processing stabilizer.
- ] is
- 3.9 (MPa) 1/2 satisfies the 1.8 to 5.5 (MPa) 1/2.
- this polyamide 12 composition is referred to as (A-2).
- ] is
- 3.9 (MPa) 1/2 satisfies the 1.8 to 5.5 (MPa) 1/2.
- ] is
- 3.9 (MPa) 1/2 satisfies the 1.8 to 5.5 (MPa) 1/2.
- Polyamide 12 Composition (A-4) The composition of the polyamide 12 was the same as that of the polyamide 12 composition (A-1), except that the polyamide 6/12 (A2-1) was changed to the polyamide 6 (A2-2).
- Polyamide 12 (A1-1) / polyamide 6 (A2-2) / elastomeric polymer (A3-1) 70.0 / 10.0 / 20 in the same manner as in the production of product (A-1).
- Pellets of a polyamide 12 composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 0 (mass ratio) were obtained (hereinafter, this polyamide 12
- the composition is called (A-4).
- Polyamide 12 Composition (A-5) In the preparation of Polyamide 12 Composition (A-1), except that the polyamide 6/12 (A2-1) was changed to the polyamide 610 (A2-3), the composition of the polyamide 12 was the same.
- Polyamide 12 (A1-1) / polyamide 610 (A2-3) / elastomeric polymer (A3-1) 70.0 / 10.0 / 20 in the same manner as in the production of product (A-1).
- Pellets of a polyamide 12 composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 0 (mass ratio) (hereinafter, this polyamide 12
- the composition is called (A-5).
- Polyamide 12 composition (A-6) A polyamide was produced in the production of Polyamide 12 composition (A-1), except that polyamide 6/12 (A2-1) was changed to polyamide 6T / 6I (A2-4).
- Polyamide 12 (A1-1) / polyamide 6T / 6I (A2-4) / elastomeric polymer (A3-1) 70.0 / 10 in the same manner as in the production of the composition (A-1).
- Pellets of a polyamide 12 composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 0 / 20.0 (mass ratio) This polyamide 12 composition is referred to as (A-6).
- ] is
- 5.3 (MPa) 1/2 satisfies the 1.8 to 5.5 (MPa) 1/2.
- Pellets of a polyamide 12 composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 0 / 10.0 / 20.0 (mass ratio) It obtained (Hereafter, this polyamide 12 composition is called (A-7).). Absolute value of difference in solubility parameter SP value between polyamide (A1) and polyamide (A2) [
- ] is
- 3.9 (MPa) 1/2 satisfies the 1.8 to 5.5 (MPa) 1/2.
- Pellets of a polyamide 612 composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to 100 parts by mass in total of 0 (mass ratio) The composition is called (A-8).
- ] is
- 2.9 (MPa) 1/2 satisfies the 1.8 to 5.5 (MPa) 1/2.
- Polyamide 12 Composition (A-9) In the production of the polyamide 12 composition (A-1), the polyamide 6/12 (A2-1) was not used, and plasticization was performed from the middle of the cylinder of the twin-screw melt kneader 12 (A1-1) / elastomer polymer (A3-1) / in the same manner as in the preparation of the polyamide 12 composition (A-1) except that benzenesulfonic acid butylamide was injected by a metering pump as a lubricant.
- 22.5-0 2 22.5 (MPa) 1/2 , and does not satisfy 1.8 or more and 5.5 or less (MPa) 1/2 .
- 22.5-0 2 22.5 (MPa) 1/2 , and does not satisfy 1.8 or more and 5.5 or less (MPa) 1/2 .
- composition (A-11)
- the composition of polyamide 12 was the same as production of polyamide 12 composition (A-1), except that polyamide 6/12 (A2-1) was changed to polyamide 1010 (A1-2).
- Polyamide 12 (A1-1) / polyamide 1010 (A1-2) / elastomeric polymer (A3-1) 80.0 / 10.0 / 10 in the same manner as in the production of compound (A-1).
- Pellets of a polyamide 12 composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 0 (mass ratio) were obtained (hereinafter, this polyamide 12
- the composition is called (A-11).
- 1.0 (MPa) 1/2 and does not satisfy 1.8 or more and 5.5 or less (MPa) 1/2 .
- this polyamide 12 composition is referred to as (A-12).
- ] is
- 3.9 (MPa) 1/2 satisfies the 1.8 to 5.5 (MPa) 1/2.
- Semi-aromatic polyamide (B1) Preparation of Semi-Aromatic Polyamide (B1-1) 2.374 kg (15.0 mol) of 1,9-nonanediamine, 2.374 kg (15.0 mol) of 2-methyl-1,8-octanediamine, and terephthalic acid 4. 939 kg (29.7 mol), 65.9 g (0.54 mol) of benzoic acid, 9.8 g (0.1% by mass relative to the raw material) of sodium hypophosphite monohydrate, and 6.0 L of distilled water was placed in an autoclave and purged with nitrogen. Stir for 30 minutes at 100 ° C. and raise the internal temperature to 190 ° C. over 2 hours.
- this semiaromatic polyamide is referred to as (B1-2)).
- this semiaromatic polyamide is referred to as (B1-5)).
- Semi-aromatic polyamide composition (B) Preparation of Semi-Aromatic Polyamide Composition (B-1)
- maleic anhydride-modified ethylene / 1-butene copolymer (A3-1) as an impact modifier, as an antioxidant
- Triethylene glycol-bis [3- (3-t-butyl-5-methyl-4-hydroxyphenyl) propionate] (manufactured by BASF Japan Ltd., IRGANOX 245)
- tris (2,4-di-) as a phosphorus-based processing stabilizer t-Butylphenyl) phosphite (manufactured by BASF Japan Ltd., IRGAFOS 168) is premixed and supplied to a twin-screw melt kneader (manufactured by Japan Steel Works, Ltd., type: TEX44) at a cylinder temperature of 220 ° C to 300 ° C.
- a pellet of a semiaromatic polyamide composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 10% by mass
- the aromatic polyamide composition is referred to as (B-4).
- a pellet of a semiaromatic polyamide composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 10% by mass
- the aromatic polyamide composition is referred to as (B-6).
- a pellet of a semiaromatic polyamide composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 10% by mass
- the aromatic polyamide composition is called (B-8).
- a pellet of a semiaromatic polyamide composition comprising 0.8 parts by mass of an antioxidant and 0.2 parts by mass of a phosphorus-based processing stabilizer with respect to a total of 100 parts by mass of 10% by mass
- the aromatic polyamide composition is referred to as (B-9).
- a semi-aromatic polyamide composition (B-9) was prepared in the same manner as in the preparation of the semi-aromatic polyamide composition (B-9) except that the semi-aromatic polyamide (B2-1) was changed to (B2-5).
- a semi-aromatic polyamide (B1-8) was prepared using, as an impact modifier, maleic anhydride-modified ethylene / 1-butene copolymer (A3-1) and ethylene / 1-butene copolymer (manufactured by Mitsui Chemicals, Inc., Tafmer A-0550), carbon black as a conductive filler (manufactured by Lion, ketjen black EC600JD), triethylene glycol-bis [3] as an antioxidant -(3-t-Butyl-5-methyl-4-hydroxyphenyl) propionate] (BASF Japan Ltd., IRGANOx 245), and tris (2,4-di-t-butylphenyl) phosphite as a phosphorus-based processing stabilizer (BASF Japan Ltd., IRGAFOS 168) is mixed beforehand, and a twin-screw melt kneader (Ja twin-screw melt kneader (Ja twin-s
- Fluorinated polymer (C) Production of Fluorinated Polymer (C-1) A polymerization vessel with a stirrer having an internal volume of 100 L was degassed to give 92.1 kg of 1-hydrotridecafluorohexane, 1,3-dichloro-1,1,2,2.
- IAH itaconic anhydride
- TFE tetrafluoroethylene
- E ethylene
- a monomer mixture gas of TFE / E: 60/40 (molar ratio) was continuously charged so that the pressure was constant during polymerization.
- an amount of (perfluoroethyl) ethylene corresponding to 2.0 mol% and an amount of IAH corresponding to 0.5 mol% were continuously charged with respect to the total number of moles of TFE and E charged during polymerization. . 5.5 hours after the initiation of polymerization, when 8.0 kg of the monomer mixed gas and 63 g of IAH were charged, the temperature in the polymerization tank was lowered to room temperature, and the pressure was changed to normal pressure by purging.
- the obtained slurry-like fluorine-containing polymer was charged into a 200 L granulation tank charged with 75.0 kg of water, and then the temperature was raised to 105 ° C. while stirring, and granulation was carried out while removing the solvent by distillation.
- the obtained granulated product was dried at 150 ° C. for 5 hours to obtain 8.3 kg of a fluorine-containing polymer.
- the granulated product was melted at 280 ° C. and a residence time of 2 minutes using an extruder to obtain a pellet of a fluorine-containing polymer (hereinafter, this fluorine-containing polymer is referred to as (C-1). ).
- conductive fluorine-containing polymer composition 100 parts by mass of fluorine-containing polymer (C-1) and 13 parts by mass of carbon black (manufactured by Electrochemical Corporation) were mixed in advance, The mixture is supplied to a shaft melt kneader (manufactured by Toshiba Machine Co., Ltd., model: TEM-48S), melt-kneaded at a cylinder temperature of 240 ° C. to 300 ° C., extruded molten resin into strands, and introduced into a water tank. The discharged strands were water-cooled, the strands were cut with a pelletizer, and dried in a dryer at 120 ° C. for 10 hours to remove moisture, to obtain pellets of a conductive fluorine-containing polymer composition (hereinafter, this conductive) (C-2).
- Fluorine-Containing Polymer (C-3) In the production of the fluorine-containing polymer (C-1), the production of the fluorine-containing polymer (C-1) is carried out except that itaconic anhydride (IAH) is not charged. In the same manner as in the above, 7.6 kg of a fluorine-containing polymer was obtained.
- the granulated product was melted at 280 ° C. and a residence time of 2 minutes using an extruder to obtain pellets of a fluorine-containing polymer (hereinafter, this fluorine-containing polymer is referred to as (C-3). ).
- TFE tetrafluoroethylene
- the granulated product was melted using an extruder at 300 ° C. for a residence time of 2 minutes to obtain a pellet of a fluorine-containing polymer (hereinafter, this fluorine-containing polymer is referred to as (C-5). ).
- Fluorinated Polymer (C-6) In the production of the fluorinated polymer (C-5), 5-norbornene-2,3-dicarboxylic acid anhydride (NAH) 0.3% by mass 1,3- 7.6 kg of fluorine-containing polymer in the same manner as in the production of the fluorine-containing polymer (C-5) except that the dichloro-1,1,2,2,3-pentafluoropropane solution is not charged I got
- the granulated product was melted using an extruder at 300 ° C. and a residence time of 2 minutes to obtain a pellet of a fluorine-containing polymer (hereinafter, this fluorine-containing polymer is referred to as (C-6). ).
- conductive fluorine-containing polymer composition (C-7) In production of conductive fluorine-containing polymer composition (C-2), fluorine-containing polymer (C-1) was used as (C-6) , 13 parts by mass of carbon black was changed to 11 parts by mass, and the cylinder temperature was changed from 300 ° C. to 320 ° C. A pellet of a conductive fluorine-containing polymer composition was obtained (hereinafter, this conductive fluorine-containing polymer composition is referred to as (C-7)).
- the composition of the fluorine-based polymer is 24.4 / 73.1 / 2.5 in the molar ratio of the polymer unit based on CTFE / the polymer unit based on TFE / the polymer unit based on PPVE, and in the fluorine-containing polymer
- the number of carbonate end groups per 1 ⁇ 10 6 carbon atoms in the main chain was 170.
- fusing point was 241 degreeC.
- the granulated product was melted using an extruder at 290 ° C. for a residence time of 2 minutes to obtain a pellet of a fluorine-containing polymer (hereinafter, this fluorine-containing polymer is referred to as (C-8). ).
- Fluorine-Containing Polymer (C-9) In the production of the fluorine-containing polymer (C-8), except that the 50% by mass di-n-propyl peroxydicarbonate methanol solution was not charged, the fluorine-containing polymer In the same manner as in the preparation of united (C-9), 29.8 kg of a fluorine-containing polymer was obtained.
- the composition of the fluorine-containing polymer is 24.4 / 73.1 / 2.5 in molar ratio of polymerized units based on CTFE / polymerized units based on TFE / polymerized units based on PPVE, and the melting point is 241 ° C. there were.
- the granulated product was melted using an extruder at 290 ° C. for a residence time of 2 minutes to obtain a pellet of a fluorine-containing polymer (hereinafter, this fluorine-containing polymer is referred to as (C-9). ).
- Example 1 Using the above-described polyamide 12 composition (A-1) and semi-aromatic polyamide composition (B-1), using a two-layer tube molding machine (Plabor, manufactured by Plastic Engineering Research Institute Co., Ltd.) (A In (1), an extrusion temperature of 270 ° C. and (B-1) were separately melted at an extrusion temperature of 300 ° C., and the discharged molten resins were merged by an adapter to form a laminated tubular body.
- A-1 an extrusion temperature of 270 ° C. and (B-1) were separately melted at an extrusion temperature of 300 ° C.
- Example 2 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-2) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 3 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-3) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 4 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-4) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 5 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-5) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 6 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-6) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 7 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-7) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 8 A laminated tube shown in Table 1 was prepared in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to the polyamide 1010 composition (A-8) in Example 1. Obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 9 In Example 1, except that the semiaromatic polyamide composition (B-1) is changed to (B-2) and the extrusion temperature of (B-2) is changed to 340 ° C., the procedure is the same as in Example 1. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 10 The procedure is the same as in Example 1 except that the semiaromatic polyamide composition (B-1) is changed to (B-3) and the extrusion temperature of (B-3) is changed to 310 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 11 The same method as in Example 1 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-4) and the extrusion temperature of (B-4) is changed to 340 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 12 In Example 1, except that the semiaromatic polyamide composition (B-1) is changed to (B-5) and the extrusion temperature of (B-5) is changed to 290 ° C., the procedure is the same as in Example 1. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 13 The same method as in Example 1 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-6) and the extrusion temperature of (B-6) is changed to 310 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 14 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the semiaromatic polyamide composition (B-1) was changed to (B-7) in Example 1. .
- the physical property measurement results of the laminated tube are shown in Table 1.
- Example 15 The same method as in Example 1 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-9) and the extrusion temperature of (B-9) is changed to 240 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 16 In Example 1, except that the semiaromatic polyamide composition (B-1) is changed to (B-10) and the extrusion temperature of (B-10) is changed to 250 ° C., the procedure is the same as in Example 1. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 17 The procedure of Example 1 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-11) and the extrusion temperature of (B-11) is changed to 260 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 18 The same method as in Example 1 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-12) and the extrusion temperature of (B-12) is changed to 320 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 19 In Example 1, except that the semiaromatic polyamide composition (B-1) is changed to (B-13) and the extrusion temperature of (B-13) is changed to 240 ° C., the procedure is the same as in Example 1. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 20 The procedure is the same as in Example 1 except that the semiaromatic polyamide composition (B-1) is changed to (B-14) and the extrusion temperature of (B-14) is changed to 320 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 21 In Example 1, except that the semiaromatic polyamide composition (B-1) was changed to the conductive semiaromatic polyamide composition (B-16) and the extrusion temperature of (B-16) was changed to 320 ° C.
- a laminated tube having a layer configuration shown in Table 1 was obtained.
- the physical property measurement results of the laminated tube are shown in Table 1.
- the conductivity of the laminated tube was measured according to SAE J-2260, and it was 10 6 ⁇ / square or less, which confirmed that the static electricity removing performance was excellent.
- Example 22 In Example 1, except that the semiaromatic polyamide composition (B-1) was changed to the conductive semiaromatic polyamide composition (B-17) and the extrusion temperature of (B-17) was changed to 270 ° C. In the same manner as in Example 1, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1. In addition, the conductivity of the laminated tube was measured according to SAE J-2260, and it was 10 6 ⁇ / square or less, which confirmed that the static electricity removing performance was excellent.
- Example 23 Using the polyamide 12 composition (A-1), the semiaromatic polyamide composition (B-1), and the conductive semiaromatic polyamide composition (B-16) shown above, Plalabor Co., Ltd.)) (A-1) is separately melted at an extrusion temperature of 270 ° C, (B-1) at an extrusion temperature of 300 ° C, and (B-16) at an extrusion temperature of 320 ° C in a three-layer tube molding machine. Then, the discharged molten resin was joined by an adapter to form a laminated tubular body.
- Example 24 In Example 23, the semiaromatic polyamide composition (B-1) is changed to (B-9), and the conductive semiaromatic polyamide composition (B-16) is changed to (B-17), (B-9)
- a laminated tube having a layer constitution shown in Table 1 was obtained in the same manner as in Example 23, except that the extrusion temperature of (B-17) was changed to 240 ° C. and 270 ° C., respectively.
- the physical property measurement results of the laminated tube are shown in Table 1.
- the conductivity of the laminated tube was measured according to SAE J-2260, and it was 10 6 ⁇ / square or less, which confirmed that the static electricity removing performance was excellent.
- Example 25 By using the polyamide 12 composition (A-1), the semiaromatic polyamide composition (B-1), and the fluorine-containing polymer (C-1) shown above, Plasor (manufactured by Plastic Engineering Laboratory Co., Ltd.) ) In a three-layer tube molding machine, (A-1) is separately melted at an extrusion temperature of 270 ° C., (B-1) at an extrusion temperature of 300 ° C., and (C-1) at an extrusion temperature of 290 ° C.
- Example 26 The procedure of Example 25 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-9) and the extrusion temperature of (B-9) is changed to 240 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 27 Example 25 except that the fluorine-containing polymer (C-1) is changed to the conductive fluorine-containing polymer (C-2) and the extrusion temperature of (C-2) is changed to 310 ° C.
- a laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in No. 25.
- the physical property measurement results of the laminated tube are shown in Table 1.
- the physical property measurement results of the laminated tube are shown in Table 1.
- the conductivity of the laminated tube was measured according to SAE J-2260, and it was 10 6 ⁇ / square or less, which confirmed that the static electricity removing performance was excellent.
- Example 28 is the same as Example 25 except that the fluorinated polymer (C-1) is changed to (C-5), and the extrusion temperature of (C-5) is changed to 310 ° C.
- the laminated tube of the layer configuration shown in Table 1 was obtained.
- the physical property measurement results of the laminated tube are shown in Table 1.
- the physical property measurement results of the laminated tube are shown in Table 1.
- Example 29 is the same as Example 25 except that the fluorinated polymer (C-1) is changed to (C-8) and the extrusion temperature of (C-8) is changed to 300 ° C.
- the laminated tube of the layer configuration shown in Table 1 was obtained.
- the physical property measurement results of the laminated tube are shown in Table 1.
- the physical property measurement results of the laminated tube are shown in Table 1.
- Example 30 The polyamide 12 composition (A-1), the semiaromatic polyamide composition (B-1), the fluorine-containing polymer (C-1) and the conductive fluorine-containing polymer (C-2) shown above are used And (A-1) at an extrusion temperature of 270 ° C., (B-1) at an extrusion temperature of 300 ° C., and (C-1) in a Plabor (Plastic Engineering Research Institute, Ltd. product) 4-layer tube molding machine. (C-2) is separately melted at an extrusion temperature of 290 ° C. and an extrusion temperature of 310 ° C., and the discharged molten resin is joined by an adapter, formed into a tube, cooled by a sizing die for size control, and taken off.
- A-1 The polyamide 12 composition (A-1), the semiaromatic polyamide composition (B-1), the fluorine-containing polymer (C-1) and the conductive fluorine-containing polymer (C-2) shown above are used And (A-1) at an
- Example 31 The procedure is the same as in Example 30, except that the semiaromatic polyamide composition (B-1) is changed to (B-9) and the extrusion temperature of (B-9) is changed to 240 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 32 Example 30 except that the conductive fluorinated polymer (C-2) is changed to the fluorinated polymer (C-3) in Example 30, and the extrusion temperature of (C-3) is changed to 290 ° C.
- a laminated tube having the layer configuration shown in Table 1 was obtained in the same manner as in No. 30.
- the physical property measurement results of the laminated tube are shown in Table 1.
- Example 33 A laminated tube shown in Table 1 was obtained by the same method as in Example 30, except that the conductive fluorine-containing polymer (C-2) was changed to (C-4) in Example 30.
- the The physical property measurement results of the laminated tube are shown in Table 1.
- the conductivity of the laminated tube was measured according to SAE J-2260, and it was 10 6 ⁇ / square or less, which confirmed that the static electricity removing performance was excellent.
- Example 34 In Example 30, the fluorine-containing polymer (C-1) is changed to (C-5), and the conductive fluorine-containing polymer (C-2) to a fluorine-containing polymer (C-6), (C A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 30, except that the extrusion temperature of -5) was changed to 310 ° C. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 35 In Example 30, the fluorine-containing polymer (C-1) was changed to (C-5), the conductive fluorine-containing polymer (C-2) to (C-7), and the extrusion of (C-5) was carried out.
- a laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 30, except that the temperature was changed to 310 ° C. and the extrusion temperature of (C-7) to 330 ° C.
- the physical property measurement results of the laminated tube are shown in Table 1.
- the conductivity of the laminated tube was measured according to SAE J-2260, and it was 10 6 ⁇ / square or less, which confirmed that the static electricity removing performance was excellent.
- Example 36 Example 30 is repeated except that the fluorine-containing polymer (C-1) is changed to (C-8) and the conductive fluorine-containing polymer (C-2) is changed to the fluorine-containing polymer (C-9) In the same manner as in Example 30, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 30 is the same as Example 30 except that the fluorine-containing polymer (C-1) is changed to (C-8) and the conductive fluorine-containing polymer (C-2) is changed to (C-10).
- a laminated tube having a layer configuration shown in Table 1 was obtained by the same method. The physical property measurement results of the laminated tube are shown in Table 1.
- the conductivity of the laminated tube was measured according to SAE J-2260, and it was 10 6 ⁇ / square or less, which confirmed that the static electricity removing performance was excellent.
- Comparative Example 1 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-9) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 2 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-10) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 3 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-11) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 4 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 1 except that the polyamide 12 composition (A-1) was changed to (A-12) in Example 1. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 5 The same method as in Example 1 is followed, except that the semiaromatic polyamide composition (B-1) is changed to (B-8) and the extrusion temperature of (B-8) is changed to 350 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 6 The same method as in Example 1 is followed, except that the semiaromatic polyamide composition (B-1) is changed to (B-15) and the extrusion temperature of (B-15) is changed to 280 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 7 A laminated tube shown in Table 1 was obtained in the same manner as in Example 25 except that the polyamide 12 composition (A-1) was changed to (A-9) in Example 25. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative Example 8 A laminated tube having a layer configuration shown in Table 1 was obtained by the same method as that of Example 25 except that the polyamide 12 composition (A-1) was changed to (A-10) in Example 25. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative Example 9 A laminated tube shown in Table 1 was obtained in the same manner as in Example 25 except that the polyamide 12 composition (A-1) was changed to (A-11) in Example 25. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 10 A laminated tube shown in Table 1 was obtained in the same manner as in Example 25 except that the polyamide 12 composition (A-1) was changed to (A-12) in Example 25. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 11 The procedure of Example 25 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-8) and the extrusion temperature of (B-8) is changed to 350 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 12 The procedure of Example 25 is repeated except that the semiaromatic polyamide composition (B-1) is changed to (B-15) and the extrusion temperature of (B-15) is changed to 280 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative Example 13 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 30, except that the polyamide 12 composition (A-1) was changed to (A-9) in Example 30. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative Example 14 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 30, except that the polyamide 12 composition (A-1) was changed to (A-10) in Example 30. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 15 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 30, except that the polyamide 12 composition (A-1) was changed to (A-11) in Example 30. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative example 16 A laminated tube having a layer configuration shown in Table 1 was obtained in the same manner as in Example 30, except that the polyamide 12 composition (A-1) was changed to (A-12) in Example 30. The physical property measurement results of the laminated tube are shown in Table 1.
- Example 30 is the same method as Example 30, except that the semiaromatic polyamide composition (B-1) is changed to (B-8) and the extrusion temperature of (B-8) is changed to 350 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Comparative Example 18 The procedure is the same as in Example 30, except that the semiaromatic polyamide composition (B-1) is changed to (B-15) and the extrusion temperature of (B-15) is changed to 280 ° C. Thus, a laminated tube having a layer configuration shown in Table 1 was obtained. The physical property measurement results of the laminated tube are shown in Table 1.
- Aliphatic polyamide compositions wherein a polyamide (A2) other than the one specified in the present invention is used, and the absolute value of the difference in solubility parameter SP value between the polyamide (A1) and the polyamide (A2) is outside the specified range of the present invention The laminated tubes of Comparative Examples 3, 9 and 15 each having a layer containing H.sub.2 were inferior in the durability of the interlayer adhesion.
- the laminated tubes of Comparative Examples 4, 10, and 16 having the layer containing the aliphatic polyamide composition in which the amount of the polyamide (A2) added was outside the defined range of the present invention were inferior in chemical resistance.
- the laminated tubes of Comparative Examples 5 to 6, 11 to 12, and 17 to 18 having a layer containing a semiaromatic polyamide composition other than specified in the present invention were inferior in interlayer adhesion and its durability. .
- the laminated tubes of Examples 1 to 37 defined in the present invention have various properties such as chemical resistance, interlayer adhesion, and their durability.
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Abstract
Description
本発明の目的は、前記問題点を解決し、薬液バリア性、低温耐衝撃性、モノマー、オリゴマーの耐溶出性といった諸特性を維持しつつ、耐薬品性、層間接着性、及びその耐久性に優れた積層チューブを提供することにある。
(a)層と(b)層とを含む2層以上の積層チューブであって、
少なくとも1組の前記(a)層と前記(b)層とは、隣接して配置され、
前記(a)層は、脂肪族ポリアミド組成物(A)を含み、
前記(b)層は、半芳香族ポリアミド組成物(B)を含み、
前記脂肪族ポリアミド組成物(A)は、ポリアミド(A1)、ポリアミド(A2)、及びエラストマー重合体(A3)を含み、
前記ポリアミド(A1)は、メチレン基数のアミド基数に対する比が8.0以上の脂肪族ポリアミドであり、前記脂肪族ポリアミド組成物(A)中に、40質量%以上90質量%以下含まれ、
前記ポリアミド(A2)は、前記ポリアミド(A1)以外のポリアミドであり、前記脂肪族ポリアミド組成物(A)中に、5質量%以上30質量%以下含まれ、
前記エラストマー重合体(A3)は、カルボキシル基及び/又は酸無水物基を有する不飽和化合物から誘導される構成単位を含有し、前記脂肪族ポリアミド組成物(A)中に、5質量%以上30質量%以下含まれ、
前記ポリアミド(A1)と前記ポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド(A1)のSP値)-(ポリアミド(A2)のSP値)|]は1.8以上5.5以下(MPa)1/2であり、
前記半芳香族ポリアミド組成物(B)は、半芳香族ポリアミド(B1)又は半芳香族ポリアミド(B2)を含み、
前記半芳香族ポリアミド組成物(B)中に、前記半芳香族ポリアミド(B1)又は前記半芳香族ポリアミド(B2)が60質量%以上含まれ、
前記半芳香族ポリアミド(B1)は、前記半芳香族ポリアミド(B1)の全ジアミン単位に対して、炭素原子数9又は10の脂肪族ジアミン単位を50モル%以上含み、前記半芳香族ポリアミド(B1)の全ジカルボン酸単位に対して、テレフタル酸単位及び/又ナフタレンジカルボン酸単位を50モル%以上含み、
前記半芳香族ポリアミド(B2)は、前記半芳香族ポリアミド(B2)の全ジアミン単位に対して、キシリレンジアミン単位及び/又はビス(アミノメチル)ナフタレン単位を50モル%以上含み、前記半芳香族ポリアミド(B2)の全ジカルボン酸単位に対して、炭素原子数9又は10の脂肪族ジカルボン酸単位を50モル%以上含む積層チューブである。
[1]前記ポリアミド(A1)が、ポリヘキサメチレンドデカミド(ポリアミド612)、ポリノナメチレンドデカミド(ポリアミド912)、ポリデカメチレンセバカミド(ポリアミド1010)、ポリデカメチレンドデカミド(ポリアミド1012)、ポリドデカメチレンドデカミド(ポリアミド1212)、ポリウンデカンアミド(ポリアミド11)、及びポリドデカンアミド(ポリアミド12)からなる群より選ばれる少なくとも1種の単独重合体、並びに/又はこれらを形成する原料単量体を数種用いた共重合体である積層チューブ。
[2]前記ポリアミド(A2)が、ポリカプロアミド(ポリアミド6)、ポリヘキサメチレンアジパミド(ポリアミド66)、ポリヘキサメチレンアゼラミド(ポリアミド69)、ポリヘキサメチレンセバカミド(ポリアミド610)、ポリヘキサメチレンテレフタラミド(ポリアミド6T)、ポリヘキサメチレンイソフタラミド(ポリアミド6I)、及びポリメタキシリレンアジパミド(ポリアミドMXD6)からなる群より選ばれる少なくとも1種の単独重合体、並びに/若しくはこれらを形成する原料単量体を数種用いた共重合体、又は、前記ポリカプロアミド(ポリアミド6)、ポリヘキサメチレンアジパミド(ポリアミド66)、ポリヘキサメチレンアゼラミド(ポリアミド69)、ポリヘキサメチレンセバカミド(ポリアミド610)、ポリヘキサメチレンテレフタラミド(ポリアミド6T)、ポリヘキサメチレンイソフタラミド(ポリアミド6I)、及びポリメタキシリレンアジパミド(ポリアミドMXD6)からなる群より選ばれる少なくとも1種を形成する原料単量体を主成分とし、ポリヘキサメチレンドデカミド(ポリアミド612)、ポリノナメチレンドデカミド(ポリアミド912)、ポリデカメチレンセバカミド(ポリアミド1010)、ポリデカメチレンドデカミド(ポリアミド1012)、ポリドデカメチレンドデカミド(ポリアミド1212)、ポリウンデカンアミド(ポリアミド11)、及びポリドデカンアミド(ポリアミド12)からなる群より選ばれる少なくとも1種を形成する原料単量体を数種用いた共重合体である積層チューブ。
[3]前記脂肪族ポリアミド組成物(A)中の前記ポリアミド(A1)及び前記ポリアミド(A2)それぞれにおける1gあたりの末端アミノ基濃度を[A](μeq/g)、末端カルボキシル基濃度を[B](μeq/g)とした時、[A]>[B]+10である積層チューブ。
[4]前記半芳香族ポリアミド組成物(B)が、前記エラストマー重合体(A3)を含む積層チューブ。
[5]前記(b)層が、前記(a)層に対して内側に隣接して配置される積層チューブ。
[6]更に(c)層を含み、
少なくとも1組の前記(b)層と前記(c)層とが隣接して配置され、
前記(c)層は、アミノ基に対して反応性を有する官能基が分子鎖中に導入された含フッ素系重合体(C)を含む積層チューブ。
[7]前記(c)層が、前記(b)層に対して内側に配置される積層チューブ。
[8]最内層が、導電性フィラーを含有させた熱可塑性樹脂組成物を含む導電層である積層チューブ。
[9]共押出成形により製造される積層チューブ。
[10]燃料チューブとして使用される積層チューブ。
積層チューブの(a)層は、脂肪族ポリアミド組成物(A)を含む。
脂肪族ポリアミド組成物(A)は、ポリアミド(A1)、ポリアミド(A2)、及びエラストマー重合体(A3)を含み、ポリアミド(A1)は、メチレン基数のアミド基数に対する比が8.0以上の脂肪族ポリアミドであり、脂肪族ポリアミド組成物(A)中に、40質量%以上90質量%以下含まれ、ポリアミド(A2)は、前記ポリアミド(A1)以外のポリアミドであり、脂肪族ポリアミド組成物(A)中に、5質量%以上30質量%以下含まれ、エラストマー重合体(A3)は、カルボキシル基及び/又は酸無水物基を有する不飽和化合物から誘導される構成単位を含有し、脂肪族ポリアミド組成物(A)中に、5質量%以上30質量%以下含まれ、前記ポリアミド(A1)と前記ポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド(A1)のSP値)-(ポリアミド(A2)のSP値)|]は1.8以上5.5以下(MPa)1/2である(以下、脂肪族ポリアミド組成物(A)と称する場合がある。)。
また、脂肪族ポリアミド組成物(A)は、長時間燃料に接触・浸漬した後及び/又は熱処理後等における層間接着性の耐久性の観点から可塑剤を含有しないほうが好ましい。
ポリアミド(A1)は、脂肪族基のみを繰り返し単位中に含み、主鎖中にアミド結合(-CONH-)を有し、メチレン基数([CH2])とアミド基数([NHCO])の比[CH2]/[NHCO](以下、メチレン基数のアミド基数に対する比を[CH2]/[NHCO]と称する場合がある。)が8.0以上である(以下、ポリアミド(A1)と称する場合がある。)。
メチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0以上のポリアミド(A1)としては、ポリウンデカンアミド(ポリアミド11):[CH2]/[NHCO]=10.0、ポリドデカンアミド(ポリアミド12):[CH2]/[NHCO]=11.0、ポリヘキサメチレンドデカミド(ポリアミド612):[CH2]/[NHCO]=8.0、ポリヘキサメチレンテトラデカミド(ポリアミド614):[CH2]/[NHCO]=9.0、ポリヘキサメチレンヘキサデカミド(ポリアミド616):[CH2]/[NHCO]=10.0、ポリヘキサメチレンオクタデカミド(ポリアミド618):[CH2]/[NHCO]=11.0、ポリノナメチレンアゼラミド(ポリアミド99):[CH2]/[NHCO]=8.0、ポリノナメチレンセバカミド(ポリアミド910):[CH2]/[NHCO]=8.5、ポリノナメチレンドデカミド(ポリアミド912):[CH2]/[NHCO]=9.5、ポリデカメチレンスベラミド(ポリアミド108):[CH2]/[NHCO]=8.0、ポリデカメチレンアゼラミド(ポリアミド109):[CH2]/[NHCO]=8.5、ポリデカメチレンセバカミド(ポリアミド1010):[CH2]/[NHCO]=9.0、ポリデカメチレンドデカミド(ポリアミド1012):[CH2]/[NHCO]=10.0、ポリドデカメチレンアジパミド(ポリアミド126):[CH2]/[NHCO]=8.0、ポリドデカメチレンスベラミド(ポリアミド128):[CH2]/[NHCO]=9.0、ポリドデカメチレンアゼラミド(ポリアミド129):[CH2]/[NHCO]=9.5、ポリドデカメチレンセバカミド(ポリアミド1210):[CH2]/[NHCO]=10.0、ポリドデカメチレンドデカミド(ポリアミド1212):[CH2]/[NHCO]=11.0等が挙げられる。これら、ポリアミド(A1)は前記の少なくとも1種の単独重合体のみならず、これらを形成する原料単量体を数種用いた共重合体も挙げられる。
また、ポリ(ドデカンアミド/ヘキサメチレンドデカミド)共重合体(ポリアミド12/612)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は、構成繰り返し単位のモル比により変わる。ポリドデカンアミド(ポリアミド12)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は11.0であり、ポリヘキサメチレンドデカミド(ポリアミド612)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は8.0であることから、構成単位の繰り返し単位のモル比が分かれば、算出可能で、ドデカンアミド単位/ヘキサメチレンドデカミド単位が80:20(質量比)、86.3:13.7(モル比)の場合、メチレン基数のアミド基数に対する比[CH2]/[NHCO]は、11.0×0.863+8.0×0.137=10.6となる。ヘキサメチレンドデカミド単位のモル比が増加すれば、メチレン基数のアミド基数に対する比[CH2]/[NHCO]は減少するが、少なくともメチレン基数のアミド基数に対する比[CH2]/[NHCO]は8.0を下回ることはない。即ち、ポリ(ドデカンアミド/ドデカメチレンドデカミド)共重合体(ポリアミド12/1212)やポリ(ドデカンアミド/ヘキサメチレンドデカミド)共重合体(ポリアミド12/612)のように、メチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0以上の脂肪族ポリアミドを形成する原料単量体(構成繰り返し単位)を数種用いた共重合体は、構成繰り返し単位のモル比によらず、メチレン基数のアミド基数に対する比[CH2]/[NHCO]は8.0以上となり、本願のポリアミド(A1)に包含される。
メチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0未満の脂肪族ポリアミドとしては、ポリカプロアミド(ポリアミド6):[CH2]/[NHCO]=5.0、ポリエチレンアジパミド(ポリアミド26):[CH2]/[NHCO]=3.0、ポリテトラメチレンスクシナミド(ポリアミド44):[CH2]/[NHCO]=3.0、ポリテトラメチレングルタミド(ポリアミド45):[CH2]/[NHCO]=3.5、ポリテトラメチレンアジパミド(ポリアミド46):[CH2]/[NHCO]=4.0、ポリテトラメチレンスベラミド(ポリアミド48):[CH2]/[NHCO]=5.0、ポリテトラメチレンアゼラミド(ポリアミド49):[CH2]/[NHCO]=5.5、ポリテトラメチレンセバカミド(ポリアミド410):[CH2]/[NHCO]=6.0、ポリテトラメチレンドデカミド(ポリアミド412):[CH2]/[NHCO]=7.0、ポリペンタメチレンスクシナミド(ポリアミド54):[CH2]/[NHCO]=3.5、ポリペンタメチレングルタミド(ポリアミド55):[CH2]/[NHCO]=4.0、ポリペンタメチレンアジパミド(ポリアミド56):[CH2]/[NHCO]=4.5、ポリペンタメチレンスベラミド(ポリアミド58):[CH2]/[NHCO]=5.5、ポリペンタメチレンアゼラミド(ポリアミド59):[CH2]/[NHCO]=6.0、ポリペンタメチレンセバカミド(ポリアミド510):[CH2]/[NHCO]=6.5、ポリペンタメチレンドデカミド(ポリアミド512):[CH2]/[NHCO]=7.5、ポリヘキサメチレンスクシナミド(ポリアミド64):[CH2]/[NHCO]=4.0、ポリヘキサメチレングルタミド(ポリアミド65):[CH2]/[NHCO]=4.5、ポリヘキサメチレンアジパミド(ポリアミド66):[CH2]/[NHCO]=5.5、ポリヘキサメチレンスベラミド(ポリアミド68):[CH2]/[NHCO]=6.0、ポリヘキサメチレンアゼラミド(ポリアミド69):[CH2]/[NHCO]=6.5、ポリヘキサメチレンセバカミド(ポリアミド610):[CH2]/[NHCO]=7.0、ポリノナメチレンアジパミド(ポリアミド96):[CH2]/[NHCO]=6.5、ポリノナメチレンスベラミド(ポリアミド98):[CH2]/[NHCO]=7.5、ポリデカメチレンアジパミド(ポリアミド106):[CH2]/[NHCO]=7.0等が挙げられる。
一方、ドデカンアミド単位/カプロアミド単位が60:40(質量比)、46.3:53.7(モル比)の場合、メチレン基数のアミド基数に対する比[CH2]/[NHCO]は、11.0×0.463+5.0×0.537=7.8となり、メチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0未満であるため、本願のポリアミド(A1)に包含されない。
このように、メチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0以上の脂肪族ポリアミドを形成する原料単量体(繰り返し単位)を一成分とし、メチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0未満の脂肪族ポリアミドを形成する原料単量体(繰り返し単位)を数種用いた共重合体におけるメチレン基数のアミド基数に対する比[CH2]/[NHCO]は、構成繰り返し単位のモル比と各ポリアミドのメチレン基数のアミド基数に対する比[CH2]/[NHCO]とにより計算可能で、メチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0以上を満たす該共重合体は本願のポリアミド(A1)に包含される。
ポリアミド(A2)は、ポリアミド(A1)以外のポリアミドであって、主鎖中にアミド結合(-CONH-)を有し、ポリアミドを形成する原料単量体(繰り返し単位)であるラクタム、アミノカルボン酸、又はジアミンとジカルボン酸を溶融重合、溶液重合、及び固相重合等の公知の方法で重合、又は共重合することにより得られる(以下、ポリアミド(A2)と称する場合がある。)。即ち、ポリアミド(A2)は脂環式ポリアミド、半芳香族ポリアミド、及びメチレン基数のアミド基数に対する比[CH2]/[NHCO]が8.0未満の脂肪族ポリアミドからなる群より選ばれる少なくとも1種である。
更に、ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド(A1)のSP値)-(ポリアミド(A2)のSP値)|]は1.8以上5.5以下(MPa)1/2であり、2.0以上5.3以下(MPa)1/2であることが好ましく、2.2以上5.0以下(MPa)1/2であることがより好ましい。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値が前記の値未満であると、得られる積層チューブの層間接着性及びその耐久性が劣ることがあり、一方、前記の値を超えると、得られる積層チューブの機械的特性及び耐薬品性が劣ることがある。
尚、溶解性パラメーターSP値は、下記に示すFedorsの式より求められる値であり、分子凝集エネルギー密度の平方根で表される値で、単位は(MPa)1/2、25℃における値である(以下、溶解性パラメーターをSP値と称する場合がある。)。
δ=[ΔEv/ΔV]1/2=[ΣΔei/ΣΔvi]1/2
δ:溶解性パラメーターSP値
ΔEv:凝集エネルギー
ΔV:モル分子容
Δei:i成分の原子又は原子団のモル凝集エネルギー
Δvi:i成分の原子又は原子団の分子容
ここで、ΔEv及びΔVはそれぞれΔEv=ΣΔei及びΔV=ΣΔviで表され、ei及びviはPOLYMER ENGINEERING AND SCIENCE(1974年発刊、第14巻、NO.2、147~154頁)より求めた値である。以下、本明細書中において記載されるSP値は、単位を(MPa)1/2とした値である。
好ましい例として挙げられている夫々のポリアミド(A1)の溶解性パラメーターSP値は(単位は(MPa)1/2)、ポリウンデカンアミド(ポリアミド11,SP値:22.9)、ポリドデカンアミド(ポリアミド12,SP値:22.5)、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)、ポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)、ポリノナメチレンデカミド(ポリアミド910,SP値:23.8)、ポリノナメチレンドデカミド(ポリアミド912,SP値:23.2)、ポリデカメチレンセバカミド(ポリアミド1010,SP値:23.5)、ポリデカメチレンドデカミド(ポリアミド1012,SP値:22.9)、ポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)となる。
前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、前記ポリアミド(A2)の中でも最低の溶解性パラメーターSP値を有するポリペンタメチレンドデカミド(ポリアミド512,SP値:24.5)やポリドデカメチレングルタミド(ポリアミド125,SP値:24.5)との溶解性パラメーターSP値の差の絶対値は2.0(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリペンタメチレンドデカミド(ポリアミド512,SP値:24.5)やポリドデカメチレングルタミド(ポリアミド125,SP値:24.5)の組み合わせは本願の規定範囲内である。
一方、前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、前記ポリアミド(A2)の中でも最低の溶解性パラメーターSP値を有するポリペンタメチレンドデカミド(ポリアミド512,SP値:24.5)やポリドデカメチレングルタミド(ポリアミド125,SP値:24.5)との溶解性パラメーターSP値の差の絶対値は0.4(MPa)1/2となり、本願の規定範囲外である。従って、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリペンタメチレンドデカミド(ポリアミド512,SP値:24.5)やポリドデカメチレングルタミド(ポリアミド125,SP値:24.5)の組み合わせは本願の規定範囲外であり、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、溶解性パラメーターSP値の差の絶対値が1.8(MPa)1/2以上となるためには、溶解性パラメーターSP値が25.9(MPa)1/2以上のポリアミド(A2)を選択する必要がある。
また、前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、前記ポリアミド(A2)の中でも最高の溶解性パラメーターSP値を有するポリテトラメチレンアジパミド(ポリアミド46,SP値:28.3)の溶解性パラメーターSP値の差の絶対値は5.8(MPa)1/2となり、本願の規定範囲外である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリテトラメチレンアジパミド(ポリアミド46,SP値:28.3)の組み合わせは本願の規定範囲外であり、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、溶解性パラメーターSP値の差の絶対値が5.5(MPa)1/2以下となるためには、溶解性パラメーターSP値が28.0(MPa)1/2以下のポリアミド(A2)を選択する必要がある。
一方、前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、前記ポリアミド(A2)の中でも最高の溶解性パラメーターSP値を有するポリテトラメチレンアジパミド(ポリアミド46,SP値:28.3)の溶解性パラメーターSP値の差の絶対値は4.2(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリテトラメチレンアジパミド(ポリアミド46,SP値:28.3)の組み合わせは本願の規定範囲内である。
これらの中でも、ポリカプロアミド(ポリアミド6)、ポリヘキサメチレンアジパミド(ポリアミド66)、ポリヘキサメチレンアゼラミド(ポリアミド69)、ポリヘキサメチレンセバカミド(ポリアミド610)、ポリ(カプロアミド/ヘキサメチレンアジパミド)共重合体(ポリアミド6/66)、ポリ(カプロアミド/ヘキサメチレンアゼラミド)共重合体(ポリアミド6/69)、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610)、ポリ(カプロアミド/ヘキサメチレンドデカミド)共重合体(ポリアミド6/612)、ポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12)、ポリ(カプロアミド/ヘキサメチレンアジパミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/66/610)、ポリ(カプロアミド/ヘキサメチレンアジパミド/ヘキサメチレンドデカミド)共重合体(ポリアミド6/66/612)、ポリ(カプロアミド/ヘキサメチレンアジパミド/ドデカンアミド)共重合体(ポリアミド6/66/12)、ポリ(カプロアミド/ヘキサメチレンセバカミド/ドデカンアミド)共重合体(ポリアミド6/610/12)、ポリ(カプロアミド/ヘキサメチレンドデカミド/ドデカンアミド)共重合体(ポリアミド6/612/12)がより好ましく、ポリカプロアミド(ポリアミド6)、ポリヘキサメチレンセバカミド(ポリアミド610)、ポリ(カプロアミド/ヘキサメチレンアジパミド)共重合体(ポリアミド6/66)、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610)、ポリ(カプロアミド/ヘキサメチレンドデカミド)共重合体(ポリアミド6/612)、ポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12)、ポリ(カプロアミド/ヘキサメチレンアジパミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/66/610)、ポリ(カプロアミド/ヘキサメチレンアジパミド/ヘキサメチレンドデカミド)共重合体(ポリアミド6/66/612)、ポリ(カプロアミド/ヘキサメチレンアジパミド/ドデカンアミド)共重合体(ポリアミド6/66/12)が更に好ましい。
例えば、ポリ(カプロアミド/ヘキサメチレンアジパミド)共重合体(ポリアミド6/66)の溶解性パラメーターSP値は、ポリカプロアミド(ポリアミド6)とポリヘキサメチレンアジパミド(ポリアミド66)の溶解性パラメーターSP値は26.9(MPa)1/2であることから、構成繰り返し単位の質量比、モル比にかかわらず、溶解性パラメーターSP値は26.9(MPa)1/2である。
前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、ポリ(カプロアミド/ヘキサメチレンアジパミド)共重合体(ポリアミド6/66)の構成繰り返し単位の質量比、モル比にかかわらず、SP値は26.9(MPa)1/2であることから、溶解性パラメーターSP値の差の絶対値は2.8(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリ(カプロアミド/ヘキサメチレンアジパミド)共重合体(ポリアミド6/66,SP値:26.9)の組み合わせは本願の規定範囲内である。
一方、前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、ポリ(カプロアミド/ヘキサメチレンアジパミド)共重合体(ポリアミド6/66)の構成繰り返し単位の質量比、モル比にかかわらず、SP値は26.9(MPa)1/2であることから、溶解性パラメーターSP値の差の絶対値は4.4(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリ(カプロアミド/ヘキサメチレンアジパミド)共重合体(ポリアミド6/66,SP値:26.9)の組み合わせは本願の規定範囲内である。
このポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=85.2/14.8モル%)に対して、前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、溶解性パラメーターSP値の差の絶対値は2.5(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=85.2/14.8モル%,SP値:26.6)の組み合わせは本願の規定範囲内である。
一方、このポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=85.2/14.8モル%)に対して、前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、溶解性パラメーターSP値の差の絶対値は4.1(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=85.2/14.8モル%,SP値:26.6)の組み合わせは本願の規定範囲内である。
次に、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610)において、カプロアミド単位/ヘキサメチレンセバカミド単位が30:70(質量比)、38.1/61.9(モル比)の場合、溶解性パラメーターSP値は、26.9×0.381+24.9×0.619=25.7(MPa)1/2となる。
このポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=38.1/61.9モル%)に対して、前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、溶解性パラメーターSP値の差の絶対値は1.6(MPa)1/2となり、本願の規定範囲外である。従って、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=38.1/61.9モル%,SP値:25.7)の組み合わせは本願の規定範囲外である。
一方、このポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=38.1/61.9モル%)に対して、前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、溶解性パラメーターSP値の差の絶対値は3.2(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/610=38.1/61.9モル%,SP値:25.7)の組み合わせは本願の規定範囲内である。
このポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12=87.5/12.5モル%)に対して、前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、溶解性パラメーターSP値の差の絶対値は2.3(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12=87.5/12.5モル%,SP値:26.4)の組み合わせは本願の規定範囲内である。
一方、このポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12=87.5/12.5モル%)に対して、前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、溶解性パラメーターSP値の差の絶対値は3.9(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12=87.5/12.5モル%,SP値:26.4)の組み合わせは本願の規定範囲内である。
次に、ポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12)において、カプロアミド単位/ドデカンアミド単位が60:40(質量比)、72.3/27.7(モル比)の場合、溶解性パラメーターSP値は、26.9×0.723+22.5×0.277=25.7(MPa)1/2となる。
このポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12=72.3/27.7モル%)に対して、前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、溶解性パラメーターSP値の差の絶対値は1.6(MPa)1/2となり、本願の規定範囲外である。従って、ポリアミド(A1)として、ポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12=72.3/27.7モル%,SP値:25.7)の組み合わせは本願の規定範囲外である。
一方、このポリ(カプロアミド/ドデカンアミド)共重合体(ポリアミド6/12=72.3/27.7モル%)に対して、前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、溶解性パラメーターSP値の差の絶対値は3.2(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリ(カプロアミド/ヘキサメチレンセバカミド)共重合体(ポリアミド6/12=72.3/27.7モル%,SP値:25.7)の組み合わせは本願の規定範囲内である。
前記ポリアミド(A1)の中でも最高の溶解性パラメーターSP値を有するポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)が選択される場合、ポリ(ヘキサメチレンテレフタラミド/ヘキサメチレンイソフタラミド)共重合体(ポリアミド6T/6I)の構成繰り返し単位の質量比、モル比にかかわらず、溶解性パラメーターSP値は27.8(MPa)1/2であることから、溶解性パラメーターSP値の差の絶対値は3.7(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)としてポリヘキサメチレンドデカミド(ポリアミド612,SP値:24.1)やポリノナメチレンアゼラミド(ポリアミド99,SP値:24.1)とポリアミド(A2)として、ポリ(ヘキサメチレンテレフタラミド/ヘキサメチレンイソフタラミド)共重合体(ポリアミド6T/6I,SP値:27.8)の組み合わせは本願の規定範囲内である。一方、前記ポリアミド(A1)の中でも最低の溶解性パラメーターSP値を有するポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)が選択される場合、ポリ(ヘキサメチレンテレフタラミド/ヘキサメチレンイソフタラミド)共重合体(ポリアミド6T/6I)の構成繰り返し単位の質量比、モル比にかかわらず、SP値は27.8(MPa)1/2であることから、溶解性パラメーターSP値の差の絶対値は5.3(MPa)1/2となり、本願の規定範囲内である。従って、ポリアミド(A1)として、ポリドデカンアミド(ポリアミド12,SP値:22.5)やポリドデカメチレンドデカミド(ポリアミド1212,SP値:22.5)とポリアミド(A2)として、ポリ(ヘキサメチレンテレフタラミド/ヘキサメチレンイソフタラミド)共重合体(ポリアミド6T/6I,SP値:27.8)の組み合わせは本願の規定範囲内である。
前記アミン類としてはモノアミン、ジアミン、トリアミン、ポリアミンが挙げられる。また、アミン類の他に、前記の末端基濃度条件の範囲を外れない限り、必要に応じて、モノカルボン酸、ジカルボン酸、トリカルボン酸等のカルボン酸類を添加しても良い。これら、アミン類、カルボン酸類は、同時に添加しても、別々に添加しても良い。また、下記例示のアミン類、カルボン酸類は、1種又は2種以上を用いることができる。
エラストマー重合体(A3)としては、(エチレン及び/又はプロピレン)/α-オレフィン系共重合体、(エチレン及び/又はプロピレン)/(α,β-不飽和カルボン酸エステル)系共重合体、芳香族ビニル化合物/共役ジエン化合物系ブロック共重合体が挙げられ、これらは1種又は2種以上を用いることができる。
芳香族ビニル化合物/共役ジエン化合物系ブロック共重合体及びその水素添加物の分子構造は、直鎖状、分岐状、放射状、又はそれら任意の組み合わせのいずれであってもよい。これらの中でも、芳香族ビニル化合物/共役ジエン化合物系ブロック共重合体及び/又はその水素添加物として、1個の芳香族ビニル化合物重合体ブロックと1個の共役ジエン化合物系重合体ブロックが直鎖状に結合したジブロック共重合体、芳香族ビニル化合物系重合体ブロック-共役ジエン化合物系重合体ブロック-芳香族ビニル化合物系重合体ブロックの順に3つの重合体ブロックが直鎖状に結合しているトリブロック共重合体、及びそれらの水素添加物の1種又は2種以上が好ましく用いられ、未水添又は水添スチレン/ブタジエンブロック共重合体、未水添又は水添スチレン/イソプレンブロック共重合体、未水添又は水添スチレン/ブタジエン/スチレンブロック共重合体、未水添又は水添スチレン/イソプレン/スチレンブロック共重合体、未水添又は水添スチレン/(エチレン/ブタジエン)/スチレンブロック共重合体、未水添又は水添スチレン/(イソプレン/ブタジエン)/スチレンブロック共重合体等が挙げられる。
積層チューブの(b)層は、半芳香族ポリアミド組成物(B)を含む。
[半芳香族ポリアミド組成物(B)]
半芳香族ポリアミド組成物(B)は、半芳香族ポリアミド(B1)又は半芳香族ポリアミド(B2)を含み、前記半芳香族ポリアミド組成物(B)中に、前記半芳香族ポリアミド(B1)又は前記半芳香族ポリアミド(B2)が60質量%以上含まれ、半芳香族ポリアミド(B1)は、芳香族ポリアミド(B1)の全ジアミン単位に対して、炭素原子数9又は10の脂肪族ジアミン単位を50モル%以上含み、半芳香族ポリアミド(B1)の全ジカルボン酸単位に対して、テレフタル酸単位及び/又ナフタレンジカルボン酸単位を50モル%以上含み、半芳香族ポリアミド(B2)は、半芳香族ポリアミド(B2)の全ジアミン単位に対して、キシリレンジアミン単位及び/又はビス(アミノメチル)ナフタレン単位を50モル%以上含み、半芳香族ポリアミド(B2)の全ジカルボン酸単位に対して、炭素原子数9又は10の脂肪族ジカルボン酸単位を50モル%以上含む(以下、半芳香族ポリアミド組成物(B)と称する場合がある。)。
半芳香族ポリアミド組成物(B)は、半芳香族ポリアミド(B1)を含む態様があり(以下、半芳香族ポリアミド(B1)と称する場合がある。)、半芳香族ポリアミド(B1)は、半芳香族ポリアミド(B1)の全ジアミン単位に対して、炭素原子数9又は10の脂肪族ジアミン単位を50モル%以上含むジアミン単位と、半芳香族ポリアミド(B1)の全ジカルボン酸単位に対して、テレフタル酸単位及び/又ナフタレンジカルボン酸単位を50モル%以上含むジカルボン酸単位を含有する。
半芳香族ポリアミド組成物(B)は、半芳香族ポリアミド(B2)を含む態様があり(以下、半芳香族ポリアミド(B2)と称する場合がある。)、半芳香族ポリアミド(B2)は、半芳香族ポリアミド(B2)の全ジアミン単位に対して、キシリレンジアミン単位及び/又はビス(アミノメチル)ナフタレン単位を50モル%以上含むジアミン単位と、半芳香族ポリアミド(B2)の全ジカルボン酸単位に対して、炭素原子数9又は10の脂肪族ジカルボン酸単位を50モル%以上含むジカルボン酸単位を含有する。
リン原子含有化合物としては、ホスフィン酸(次亜リン酸)、次亜リン酸エチル、ジメチルホスフィン酸、フェニルメチルホスフィン酸、次亜リン酸ナトリウム、次亜リン酸カリウム、次亜リン酸リチウム、次亜リン酸カルシウム、次亜リン酸マグネシウム、亜リン酸、亜リン酸トリエチル、亜リン酸トリフェニル、亜リン酸ナトリウム、亜リン酸水素ナトリウム、亜リン酸カリウム、亜リン酸水素カリウム、亜リン酸リチウム、亜リン酸水素リチウム、亜リン酸マグネシウム、亜リン酸水素マグネシウム、亜リン酸カルシウム、亜リン酸水素カルシウム、ピロ亜リン酸、リン酸、リン酸ナトリウム、リン酸水素二ナトリウム、リン酸二水素ナトリウム、リン酸カリウム、リン酸水素二カリウム、リン酸二水素カリウム、リン酸マグネシウム、リン酸水素二マグネシウム、リン酸二水素マグネシウム、リン酸カルシウム、リン酸水素二カルシウム、リン酸二水素カルシウム、リン酸リチウム、リン酸水素二リチウム、リン酸二水素リチウム、ピロリン酸ナトリウム、ピロリン酸カリウム、ピロリン酸マグネシウム、ピロリン酸カルシウム、ピロリン酸リチウム、メタリン酸ナトリウム、メタリン酸カリウム、メタリン酸マグネシウム、メタリン酸カルシウム、メタリン酸リチウム、亜ホスホン酸、亜ホスホン酸ナトリウム、亜ホスホン酸リチウム、亜ホスホン酸カリウム、亜ホスホン酸マグネシウム、亜ホスホン酸カルシウム、フェニル亜ホスホン酸エチル、フェニル亜ホスホン酸ナトリウム、フェニル亜ホスホン酸カリウム、フェニル亜ホスホン酸リチウム、ホスホン酸、ホスホン酸ナトリウム、ホスホン酸カリウム、ホスホン酸リチウム、ホスホン酸カリウム、ホスホン酸マグネシウム、ホスホン酸カルシウム、フェニルホスホン酸、エチルホスホン酸、フェニルホスホン酸ナトリウム、フェニルホスホン酸カリウム、フェニルホスホン酸リチウム、フェニルホスホン酸ジエチル、エチルホスホン酸ナトリウム、エチルホスホン酸カリウム等が挙げられる。これらは1種又は2種以上を用いることができる。これらの中でも、次亜リン酸ナトリウム、次亜リン酸カリウム、次亜リン酸リチウム、次亜リン酸カルシウム、次亜リン酸マグネシウム、亜リン酸カルシウム、亜リン酸水素カルシウム、リン酸二水素カルシウム、亜リン酸ナトリウム、亜リン酸ナトリウム、亜リン酸水素ナトリウム、亜リン酸カリウム、亜リン酸水素カリウム、亜リン酸リチウム、亜リン酸水素リチウム、亜リン酸マグネシウム、亜リン酸水素マグネシウム、亜リン酸カルシウム、亜リン酸水素カルシウムが好ましく、次亜リン酸ナトリウム、次亜リン酸カリウム、次亜リン酸リチウム、次亜リン酸カルシウム、次亜リン酸マグネシウムがより好ましい。尚、これらのリン原子含有化合物は水和物であってもよい。
これらのリン原子含有化合物の添加方法は、半芳香族ポリアミド(B2)の原料であるナイロン塩水溶液、ジアミンもしくはジカルボン酸に添加する方法、溶融状態にあるジカルボン酸に添加する方法、溶融重合中に添加する方法等が挙げられるが、半芳香族ポリアミド(B2)中に均一に分散させることが可能であれば、いかなる方法でも良く、これらに限定されるものではない。
これらのアルカリ金属化合物又はアルカリ土類金属化合物の添加方法は、半芳香族ポリアミド(B2)の原料であるナイロン塩水溶液、ジアミンもしくはジカルボン酸に添加する方法、溶融状態にあるジカルボン酸に添加する方法、溶融重合中に添加する方法等が挙げられるが、半芳香族ポリアミド(B2)中に均一に分散させることが可能であればいかなる方法でも良く、これらに限定されるものではない。
末端封止剤の使用量は、用いる末端封止剤の反応性、沸点、反応装置、反応条件等を考慮して、適宜選択することができる。重合度の調整の観点から、原料成分であるジカルボン酸とジアミンの総モル数に対して0.1モル%以上15モル%以下であることが好ましい。
衝撃改良材の含有量は、積層チューブの機械的強度及び低温耐衝撃性を十分に確保する観点から、主成分の半芳香族ポリアミド(B1)又は半芳香族ポリアミド(B2)100質量部に対して、1質量部以上30質量部以下であることが好ましく、3質量部以上25質量部以下であることがより好ましい。
積層チューブは、更に(c)層を有することが好ましい。
積層チューブの(c)層は、アミノ基に対して反応性を有する官能基が分子鎖中に導入された含フッ素系重合体(C)(以下、含フッ素系重合体(C)と称する場合がある。)を含む。
含フッ素系重合体(C)は、アミノ基に対して反応性を有する官能基が分子鎖中に導入された含フッ素系重合体である。
含フッ素系重合体(C)は、少なくとも1種の含フッ素単量体から誘導される繰り返し単位を有する重合体(単独重合体又は共重合体)である。熱溶融加工可能な含フッ素系重合体であれば特に限定されるものではない。
ここで含フッ素単量体としては、テトラフルオロエチレン(TFE)、トリフルオロエチレン、フッ化ビニリデン(VDF)、フッ化ビニル(VF)、クロロトリフルオロエチレン(CTFE)、トリクロロフルオロエチレン、ヘキサフルオロプロピレン(HFP)、CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)、CF2=CF-OCH2-Rf2(ここで、Rf2は、炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキレン基を表す。)、CF2=CF(CF2)pOCF=CF2(ここで、pは1又は2である。)、CH2=CX1(CF2)nX2(ここで、X1及びX2は互いに独立に水素原子又はフッ素原子を表し、nは2以上10以下の整数である。)等が挙げられる。これらは1種又は2種以上を用いることができる。
これらの中でも、含フッ素系重合体(C)の薬液バリア性と耐環境応力亀裂性のバランスの観点から、CH2=CH(CF2)nF又はCH2=CF(CF2)nHで表される化合物が好ましく、式中のnは2以上4以下であることがより好ましい。
VDF単位とTFE単位とからなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、VDF単位の含有量が30モル%以上99モル%以下、及びTFE単位の含有量が1モル%以上70モル%以下である共重合体(C1-2)、
VDF単位、TFE単位、及びトリクロロフルオロエチレン単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、VDF単位の含有量が10モル%以上90モル%以下、TFE単位の含有量が0モル%以上90モル%以下、及びトリクロロフルオロエチレン単位の含有量が0モル%以上30モル%以下である共重合体(C1-3)、
VDF単位、TFE単位、及びHFP単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、VDF単位の含有量が10モル%以上90モル%以下、TFE単位の含有量が0モル%以上90モル%以下、及びHFP単位の含有量が0モル%以上30モル%以下である共重合体(C1-4)等が挙げられる。
TFE単位とE単位、及び前記一般式CH2=CX1(CF2)nX2(ここで、X1及びX2は互いに独立に水素原子又はフッ素原子を表し、nは2以上10以下の整数である。)で表されるフルオロオレフィンに由来するフルオロオレフィン単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、TFE単位の含有量が30モル%以上70モル%以下、E単位の含有量が20モル%以上55モル%以下、及び前記一般式CH2=CX3(CF2)nX4(ここで、X3及びX4は互いに独立に水素原子又はフッ素原子を表し、nは2以上10以下の整数である。)で表されるフルオロオレフィンに由来するフルオロオレフィン単位の含有量が0モル%以上10モル%以下である共重合体(C2-1)、
TFE単位とE単位とHFP単位、及びこれらと共重合可能な単量体に由来する単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、TFE単位の含有量が30モル%以上70モル%以下、E単位の含有量が20モル%以上55モル%以下、HFP単位の含有量が1モル%以上30モル%以下、及びこれらと共重合可能な単量体に由来する単位の含有量が0モル%以上10モル%以下である共重合体(C2-2)、
TFE単位とE単位、及び前記一般式CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)で表されるPAVEに由来するPAVE単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、TFE単位の含有量が30モル%以上70モル%以下、E単位の含有量が20モル%以上55モル%以下、及び前記一般式CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)で表されるPAVEに由来するPAVE単位の含有量が0モル%以上10モル%以下である共重合体(C2-3)等が挙げられる。
TFE単位及びHFP単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、TFE単位の含有量が70モル%以上95モル%以下であり、好ましくは85モル%以上93モル%以下であり、HFP単位の含有量が5モル%以上30モル%以下であり、好ましくは7モル%以上15モル%以下である共重合体(C3-1)、
TFE単位及び前記一般式CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)で表されるPAVEに由来する1種又は2種以上のPAVE単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、TFE単位の含有量が70モル%以上95モル%以下、及び前記一般式CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)で表されるPAVEに由来する1種又は2種以上のPAVE単位の含有量が5モル%以上30モル%以下である共重合体(C3-2)、
TFE単位とHFP単位、及び前記一般式CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)で表されるPAVEに由来する1種又は2種以上のPAVE単位からなる共重合体であって、後記の官能基含有単量体を除く単量体全体に対して、TFE単位の含有量が70モル%以上95モル%以下、HFP単位と前記一般式CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)で表されるPAVEに由来する1種又は2種以上のPAVE単位の合計含有量が5モル%以上30モル%以下である共重合体(C3-3)等が挙げられる。
前記CTFE共重合体(C4)における含フッ素単量体としては、CTFE以外のものであれば特に限定されないが、フッ化ビニリデン(VDF)、ヘキサフルオロプロピレン(HFP)、前記一般式CF2=CFORf1(ここで、Rf1は炭素原子数1以上10以下のエーテル性酸素原子を含んでもよいパーフルオロアルキル基を表す。)で表されるPAVE、前記一般式CH2=CX1(CF2)nX2(ここで、X1及びX2は互いに独立に水素原子又はフッ素原子を表し、nは2以上10以下の整数である。)で表されるフルオロオレフィン等が挙げられる。これらは1種又は2種以上を用いることができる。
また、重合は、一槽ないし多槽式の攪拌型重合装置、管型重合装置を使用して、回分式又は連続式操作として実施することができる。
含フッ素系重合体(C)の融点は、目的、用途、使用方法により適宜選択されるが、前記脂肪族ポリアミド組成物(A)及び半芳香族ポリアミド組成物(B)等と共押出する場合、当該樹脂の成形温度に近いことが好ましい。そのため、前記含フッ素単量体、その他の単量体と後記の官能基含有単量体の割合を適宜調節し、含フッ素系重合体(C)の融点を最適化することが好ましい。
ここで、融点とは、示差走査熱量測定装置を用いて、試料を予想される融点以上の温度に加熱し、次に、この試料を1分間あたり10℃の速度で降温し、30℃まで冷却、そのまま約1分間放置したのち1分間あたり10℃の速度で昇温することにより測定される融解曲線のピーク値の温度を融点と定義するものとする。
前記一般式におけるYであるカルボキシル基由来基としては、例えば、一般式-C(=O)Q1(式中、Q1は、-OR8、-NH2、F、Cl、Br又はIを表し、R8は、炭素原子数1以上20以下のアルキル基又は炭素原子数6以上22以下のアリール基を表す。)で表される基等が挙げられる。
前記一般式におけるYであるスルホン酸由来基としては、例えば、一般式-SO2Q2(式中Q2は、-OR9、-NH2、F、Cl、Br又はIを表し、R9は、炭素原子数1以上20以下のアルキル基又は炭素原子数6以上22以下のアリール基を表す。)で表される基等が挙げられる。
前記Yは、-COOH、-SO3H、-SO3Na、-SO2F又は-CNが好ましい。
尚、含フッ素共重合体(C)中の官能基含有単量体の含有量としては、全重合単位に対して、0.01モル%とは、含フッ素共重合体(C)中の官能基残基の含有量が含フッ素共重合体(C)の主鎖炭素数1×106個に対して100個であることに相当する。また、含フッ素共重合体(C)中の全重合単位に対して、5.0モル%とは、含フッ素共重合体(C)中の官能基残基の含有量が含フッ素共重合体(C)の主鎖炭素数1×106個に対して50,000個であることに相当する。また、前記含有量を満たす限りにおいて、官能基が導入された含フッ素系重合体と、官能基が導入されていない含フッ素系重合体の混合物であって構わない。
積層チューブの第一態様は、(a)層及び(b)層の少なくとも2層を含み、少なくとも1組の(a)層と(b)層とが隣接して配置される。
導電性フィラーは、樹脂に導電性能を付与するために添加されるすべての充填材が包含され、粒状、フレーク状、及び繊維状フィラー等が挙げられる。
これら、導電性フィラーはチタネート系、アルミ系、シラン系等の表面処理剤で表面処理を施されていてもよい。また溶融混練作業性を向上させるために造粒されたものを用いることも可能である。
また、かかる導電性フィラーは、十分な帯電防止性能を得る観点から、溶融押出物の表面固有抵抗値が108Ω/square以下であることが好ましく、106Ω/square以下であることがより好ましい。但し、前記導電性フィラーの添加は強度、流動性の悪化を招きやすい。そのため、目標とする導電レベルが得られれば、前記導電性フィラーの含有量はできるだけ少ない方が望ましい。
また、かかる導電性フィラーは、十分な帯電防止性能を得る観点から、溶融押出物の表面固有抵抗値が108Ω/square以下であることが好ましく、106Ω/square以下であることがより好ましい。但し、前記導電性フィラーの添加は強度、流動性の悪化を招きやすい。そのため、目標とする導電レベルが得られれば、前記導電性フィラーの含有量はできるだけ少ない方が望ましい。
積層チューブが、(c)層を有する場合、(c)層に対して、官能基を含有しないフッ素系重合体を含む層が内側に配置されることにより、低温耐衝撃性、薬液バリア性、及び耐環境応力亀裂性を両立することが可能であり、また、経済的にも有利である。
また、第二態様の積層チューブにおいては、溶融安定性及び成形安定性の観点から、前記例示の熱可塑性樹脂のうち、融点が290℃以下のポリエステル系樹脂、ポリアミド系樹脂、ポリチオエーテル系樹脂、ポリオレフィン系樹脂、及び官能基を含有しないフッ素系重合体を使用することが好ましい。
[相対粘度]
JIS K-6920に準じて、96%の硫酸中、ポリアミド濃度1%、温度25℃の条件下で測定した。
活栓付三角フラスコに所定量のポリアミド試料を入れ、あらかじめ調整しておいた溶媒フェノール/メタノール(体積比9/1)の40mLを加えた後、マグネットスターラで攪拌溶解し、指示薬にチモールブルーを用いて0.05Nの塩酸で滴定を行い、末端アミノ基濃度を求めた。
三つ口ナシ型フラスコに所定量のポリアミド試料を入れ、ベンジルアルコール40mLを加えた後、窒素気流下、180℃に設定したオイルバスに浸漬する。上部に取り付けた攪拌モータにより攪拌溶解し、指示薬にフェノールフタレインを用いて0.05Nの水酸化ナトリウム溶液で滴定を行い、末端カルボキシル基濃度を求めた。
三つ口ナシ型フラスコに所定量のエラストマー重合体試料を入れ、トルエン170mLに溶解し、更にエタノールを30mL加えて調製した試料溶液を用いて、フェノールフタレインを指示薬とし、0.1NのKOHエタノール溶液で滴定を行い、カルボキシル基及び酸無水物基の合計濃度を求めた。
[含フッ素系重合体の組成]
溶融NMR分析、フッ素含有量分析、赤外吸収スペクトルにより測定した。
含フッ素系重合体中の末端カーボネート基数は、赤外吸収スペクトル分析により、カーボネート基(-OC(=O)O-)のカルボニル基が帰属するピークが1810~18cm-1の吸収波長に現われ、吸収ピークの吸光度を測定し、次式によって含フッ素系重合体中の主鎖炭素原子数1×106個に対するカーボネート基の個数を算出した。
[含フッ素系重合体中の主鎖炭素原子数106個に対するカーボネート基の個数]=500AW/εdf
A:カーボネート基(-OC(=O)O-)のピークの吸光度
ε:カーボネート基(-OC(=O)O-)のモル吸光度係数[cm-1・mol-1]。モデル化合物よりε=170とした。
W:モノマー組成から計算される組成平均分子量
d:フィルムの密度[g/cm3]
f:フィルムの厚み[mm]
[耐薬品性(耐塩化亜鉛性)]
チューブ端部にポリアミド12製継手を圧入し、SAE J-2260 7.12に記載の方法で、塩化亜鉛浸漬を実施した。その後、サンプルを取り出し、クラック発生有無を確認した。その後、SAE J-2260 7.5に記載の方法で、-40℃にて衝撃試験を実施した。
200mmにカットしたチューブを更に縦方向に半分にカットし、テストピースを作成した。万能材料試験機(オリエンテック社製、テンシロンUTMIII-200)を用い、50mm/minの引張速度にて90°剥離試験を実施した。S-Sカーブの極大点から剥離強度を読み取り、層間接着性を評価した。
200mmにカットしたチューブを160℃のオーブンに入れ、30分処理した。取り出したチューブの層間接着性を前記の方法に従い評価した。熱処理後の剥離強度が3.0N/mm以上の場合、層間接着性の耐久性に優れていると判断した。
ポリアミド(A1)
ポリアミド12(A1-1)の製造
内容積70リットルの攪拌機付き耐圧力反応容器に、ドデカンラクタム19.73kg(100.0モル)、5-アミノ-1,3,3-トリメチルシクロヘキサンメチルアミン45.0g(0.264モル)、及び蒸留水0.5Lを仕込み、重合槽内を窒素置換した後、180℃まで加熱し、この温度で反応系内が均一な状態になるように攪拌した。次いで重合槽内温度を270℃まで昇温させ、槽内圧力を3.5MPaに調圧しながら、2時間攪拌下に重合した。その後、約2時間かけて常圧に放圧し、次いで、53kPaまで減圧し、減圧下において5時間重合を行なった。次いで、窒素をオートクレーブ内に導入し、常圧に復圧後、反応容器の下部ノズルからストランドとして抜き出し、カッティングしてペレットを得た。このペレットを減圧乾燥し、相対粘度2.10、末端アミノ基濃度48μeq/g、末端カルボキシル基濃度24μeq/gのポリアミド12を得た(以下、このポリアミド12を(A1-1)という。)。ポリアミド12(A1-1)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は11.0であり、8.0以上を満たす。ポリアミド12(A1-1)の溶解性パラメーターSP値は22.5(MPa)1/2である。また、ポリアミド12(A1-1)の末端アミノ基濃度[A](μeq/g)、末端カルボキシル基濃度[B](μeq/g)は、[A]>[B]+10を満たす。
内容積70リットルの攪拌機付き耐圧力反応容器に、1,10-デカンジアミンとセバシン酸の等モル塩17.82kg(50.0モル)、1,10-デカンジアミン29.3g(0.17モル)、及び蒸留水5.0Lを仕込み、重合槽内を窒素置換した後、220℃まで加熱し、この温度で反応系内が均一な状態になるように攪拌した。次いで、重合槽内温度を270℃まで昇温させ、槽内圧力を1.7MPaに調圧しながら、2時間攪拌下に重合した。その後、約2時間かけて常圧に放圧し、次いで、53kPaまで減圧し、減圧下において4時間重合を行なった。次いで、窒素をオートクレーブ内に導入し、常圧に復圧後、反応容器の下部ノズルからストランドとして抜き出し、カッティングしてペレットを得た。このペレットを減圧乾燥し、相対粘度2.22、末端アミノ基濃度45μeq/g、末端カルボキシル基濃度28μeq/gのポリアミド1010を得た(以下、このポリアミド1010を(A1-2)という。)。ポリアミド1010(A1-2)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は9.0であり、8.0以上を満たす。ポリアミド1010(A1-2)の溶解性パラメーターSP値は23.5(MPa)1/2である。また、ポリアミド1010(A1-2)の末端アミノ基濃度[A](μeq/g)、末端カルボキシル基濃度[B](μeq/g)は、[A]>[B]+10を満たす。
ポリアミド6/12(A2-1)の製造
内容積70リットルの攪拌機付き耐圧力反応容器に、カプロラクタム9.90kg(87.5モル)、12-アミノドデカン酸2.69kg(12.5モル)、5-アミノ-1,3,3-トリメチルシクロヘキサンメチルアミン20.0g(0.12モル)、及び蒸留水2.0Lを入れ、100℃に加熱し、この温度で反応系内が均一な状態になるように攪拌した。引き続き、更に温度を260℃まで昇温させ、2.5MPaの圧力下で1時間攪拌した。その後、放圧して水分を反応容器から揮散させながら常圧下、260℃で2時間重合反応を行い、更に260℃、53kPaの減圧下で4時間重合反応させた。反応終了後、反応容器の下部ノズルからストランド状に取り出した反応物を水槽に導入して冷却し、カッティングして、ペレットを得た。このペレットを熱水中に浸漬し、未反応モノマーを抽出して除去した後、減圧乾燥し、相対粘度2.63、末端アミノ基濃度54μeq/g、末端カルボキシル基濃度40μeq/gのポリアミド6/12(カプロアミド単位/ドデカンアミド単位=82.5/12.5モル%)を得た(以下、このポリアミド6/12を(A2-1)という。)。ポリアミド6/12(A2-1)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は5.75であり、8.0未満である。ポリアミド6/12(A2-1)の溶解性パラメーターSP値は26.4(MPa)1/2である。また、ポリアミド6/12(A2-1)の末端アミノ基濃度[A](μeq/g)、末端カルボキシル基濃度[B](μeq/g)は、[A]>[B]+10を満たす。
ポリアミド6/12(A2-1)の製造において、カプロラクタム9.90kg(87.5モル)、12-アミノドデカン酸2.69kg(12.5モル)をカプロラクタム11.32kg(100.0モル)に変更し、5-アミノ-1,3,3-トリメチルシクロヘキサンメチルアミン20.0g(0.12モル)を80.0g(0.47モル)に変更した以外は、ポリアミド6/12(A2-1)の製造と同様の方法にて、相対粘度2.50、末端アミノ基濃度112μeq/g、末端カルボキシル基濃度33μeq/gのポリアミド6を得た(以下、このポリアミド6を(A2-2)という。)。ポリアミド6(A2-2)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は5.0であり、8.0未満である。ポリアミド6(A2-2)の溶解性パラメーターSP値は26.9(MPa)1/2である。また、ポリアミド6(A2-2)の末端アミノ基濃度[A](μeq/g)、末端カルボキシル基濃度[B](μeq/g)は、[A]>[B]+10を満たす。
ポリアミド1010(A1-2)の製造において、1,10-デカンジアミンとセバシン酸の等モル塩17.82kg(50.0モル)を1,6-ヘキサンジアミンとセバシン酸の等モル塩15.02kg(50.0モル)、1,10-デカンジアミン29.3g(0.17モル)を1,6-ヘキサンジアミン15.1g(0.13モル)に変更した以外は、ポリアミド1010(A1-2)の製造と同様の方法にて、相対粘度2.58、末端アミノ基濃度73μeq/g、末端カルボキシル基濃度53μeq/gのポリアミド610を得た(以下、このポリアミド610を(A2-3)という。)。ポリアミド610(A2-3)のメチレン基数のアミド基数に対する比[CH2]/[NHCO]は7.0であり、8.0未満である。ポリアミド610(A2-3)の溶解性パラメーターSP値は24.9(MPa)1/2である。また、ポリアミド610(A2-3)の末端アミノ基濃度[A](μeq/g)、末端カルボキシル基濃度[B](μeq/g)は、[A]>[B]+10を満たす。
1,6-ヘキサンジアミン2.150kg(18.5モル)、イソフタル酸1.960kg(11.8モル)、テレフタル酸0.980kg(5.9モル)、酢酸11g(0.18モル)、次亜リン酸ナトリウム一水和物5.2g(前記モノマー原料に対して0.1質量部)、及び蒸留水9.0Lをオートクレーブに入れ、窒素置換した。100℃で30分間攪拌し、その後、オートクレーブ系内の圧力が1.8MPaまで加熱昇圧した。1.8MPaに到達後、系内圧力が一定となるように放圧させながら攪拌し、そのまま反応を5時間続けた後、水の留出はほとんどなくなり、この時点で系内の温度は250℃となっていた。更に、常圧に戻し、減圧を開始し、80kPaにて1時間反応させた。その後、復圧し、オートクレーブ底部より溶融ポリマーを抜き出し、冷却、ペレット化し、相対粘度1.95、明確な融点を示さず、末端アミノ基濃度50μeq/g、末端カルボキシル基濃度15μeq/gのポリアミド6T/6I(ヘキサメチレンテレフタラミド単位/ヘキサメチレンイソフタラミド単位=33/67モル%)を得た(以下、このポリアミド6T/6Iを(A2-4)という。)。同ポリアミドは、芳香族骨格を繰り返し単位として有するため、ポリアミド(A1)に該当しない。ポリアミド6T/6I(A2-4)の溶解性パラメーターSP値は27.8(MPa)1/2である。また、ポリアミド6T/6I(A2-4)の末端アミノ基濃度[A](μeq/g)、末端カルボキシル基濃度[B](μeq/g)は、[A]>[B]+10を満たす。
無水マレイン酸変性エチレン/1-ブテン共重合体(A3-1)(三井化学(株)製、タフマーMH5010、酸無水物基濃度:50μeq/g)
無水マレイン酸変性エチレン/1-ブテン共重合体(A3-2)(三井化学(株)製、タフマーMH5020、酸無水物基濃度:100μeq/g)
ポリアミド12組成物(A-1)の製造
ポリアミド12(A1-1)にポリアミド6/12(A2-1)、無水マレイン酸変性エチレン/1-ブテン共重合体(A3-1)、酸化防止剤としてトリエチレングリコール-ビス[3-(3-t-ブチル-5-メチル-4-ヒドロキシフェニル)プロピオネート](BASFジャパン社製、IRGANOX245)、及びリン系加工安定剤としてトリス(2,4-ジ-t-ブチルフェニル)ホスファイト(BASFジャパン社製、IRGAFOS168)をあらかじめ混合し、二軸溶融混練機((株)日本製鋼所製、型式:TEX44)に供給し、シリンダ温度180℃から270℃で溶融混練し、溶融樹脂をストランド状に押出した後、これを水槽に導入し、冷却、カット、真空乾燥して、ポリアミド12(A1-1)/ポリアミド6/12(A2-1)/エラストマー重合体(A3-1)=70.0/10.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-1)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド6/12(A2-1)のSP値)|]は|22.5-26.4|=3.9(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、ポリアミド12(A1-1)及びポリアミド6/12(A2-1)の添加量を変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド6/12(A2-1)/エラストマー重合体(A3-1)=75.0/5.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-2)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド6/12(A2-1)のSP値)|]は|22.5-26.4|=3.9(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、ポリアミド12(A1-1)及びポリアミド6/12(A2-1)の添加量を変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド6/12(A2-1)/エラストマー重合体(A3-1)=65.0/15.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-3)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド6/12(A2-1)のSP値)|]は|22.5-26.4|=3.9(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、ポリアミド6/12(A2-1)をポリアミド6(A2-2)に変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド6(A2-2)/エラストマー重合体(A3-1)=70.0/10.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-4)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド6(A2-2)のSP値)|]は|22.5-26.9|=4.4(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、ポリアミド6/12(A2-1)をポリアミド610(A2-3)に変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド610(A2-3)/エラストマー重合体(A3-1)=70.0/10.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-5)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド610(A2-3)のSP値)|]は|22.5-24.9|=2.4(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、ポリアミド6/12(A2-1)をポリアミド6T/6I(A2-4)に変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド6T/6I(A2-4)/エラストマー重合体(A3-1)=70.0/10.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-6)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド6T/6I(A2-4)のSP値)|]は|22.5-27.8|=5.3(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、無水マレイン酸変性エチレン/1-ブテン共重合体(A3-1)を(A3-2)に変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド6/12(A2-1)/エラストマー重合体(A3-2)=70.0/10.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-7)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド6/12(A2-1)のSP値)|]は|22.5-26.4|=3.9(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、ポリアミド12(A1-1)をポリアミド1010(A1-2)に変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド1010(A1-2)/ポリアミド6/12(A2-1)/エラストマー重合体(A3-1)=70.0/10.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド612組成物のペレットを得た(以下、このポリアミド1010組成物を(A-8)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド1010(A1-2)のSP値)-(ポリアミド6/12(A2-1)のSP値)|]は|23.5-26.4|=2.9(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
ポリアミド12組成物(A-1)の製造において、ポリアミド6/12(A2-1)を使用せず、二軸溶融混練機のシリンダの途中から、可塑剤としてベンゼンスルホン酸ブチルアミドを定量ポンプにより注入した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/エラストマー重合体(A3-1)/可塑剤=87.5/10.0/2.5(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-9)という。)。ポリアミド6/12(A2-1)を使用していないため、ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値は、便宜的に[|(ポリアミド12(A1-1)のSP値)-0]=|22.5-0|=22.5(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たさない。
ポリアミド12組成物(A-1)の製造において、ポリアミド6/12(A2-1)を使用しないこと以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/エラストマー重合体(A3-1)=90.0/10.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-10)という。)。ポリアミド6/12(A2-1)を使用していないため、ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値は、便宜的に[|(ポリアミド12(A1-1)のSP値)-0]=|22.5-0|=22.5(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たさない。
ポリアミド12組成物(A-1)の製造において、ポリアミド6/12(A2-1)をポリアミド1010(A1-2)に変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド1010(A1-2)/エラストマー重合体(A3-1)=80.0/10.0/10.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-11)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド1010(A1-2)のSP値)|]は|22.5-23.5|=1.0(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たさない。
ポリアミド12組成物(A-1)の製造において、ポリアミド12(A1-1)及びポリアミド6/12(A2-1)の添加量を変更した以外は、ポリアミド12組成物(A-1)の製造と同様の方法にて、ポリアミド12(A1-1)/ポリアミド6/12(A2-1)/エラストマー重合体(A3-1)=40.0/40.0/20.0(質量比)の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなるポリアミド12組成物のペレットを得た(以下、このポリアミド12組成物を(A-12)という。)。ポリアミド(A1)とポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド12(A1-1)のSP値)-(ポリアミド6/12(A2-1)のSP値)|]は|22.5-26.4|=3.9(MPa)1/2であり、1.8以上5.5以下(MPa)1/2を満たす。
半芳香族ポリアミド(B1-1)の製造
1,9-ノナンジアミン2.374kg(15.0モル)、2-メチル-1,8-オクタンジアミン2.374kg(15.0モル)、テレフタル酸4.939kg(29.7モル)、安息香酸65.9g(0.54モル)、次亜リン酸ナトリウム一水和物9.8g(原料に対して0.1質量%)、及び蒸留水6.0Lをオートクレーブに入れ、窒素置換した。100℃で30分間攪拌し、2時間かけて内部温度を190℃に昇温した。この時、オートクレーブは2.0MPaまで昇圧した。そのまま1時間反応を続けた後230℃に昇温し、その後2時間、230℃に温度を保ち、水蒸気を徐々に抜いて圧力を2.0MPaに保ちながら反応させた。次に、30分かけて圧力を1.0MPaまで下げ、更に1時間反応させて、プレポリマーを得た。これを、100℃、減圧下で12時間乾燥し、2mm以下の大きさまで粉砕し、210℃、0.013kPa下にて、8時間固相重合し、融点265℃、相対粘度2.38の半芳香族ポリアミド(ポリアミド9T/M8T=50/50モル%)を得た(以下、この半芳香族ポリアミドを(B1-1)という。)。
半芳香族ポリアミド(B1-1)の製造において、1,9-ノナンジアミン2.374kg(15.0モル)と2-メチル-1,8-オクタンジアミン2.374kg(15.0モル)を1,9-ノナンジアミン4.036kg(25.5モル)と2-メチル-1,8-オクタンジアミン0.712kg(4.5モル)に変え、固相重合温度を210から240℃に変更した以外は、半芳香族ポリアミド(B1-1)の製造と同様の方法にて、融点305℃、相対粘度2.34の半芳香族ポリアミド(ポリアミド9T/M8T=85/15モル%)を得た(以下、この半芳香族ポリアミドを(B1-2)という。)。
半芳香族ポリアミド(B1-1)の製造において、テレフタル酸4.939kg(29.7モル)を2,6-ナフタレンジカルボン酸6.427kg(29.7モル)に変更した以外は、半芳香族ポリアミド(B1-1)の製造と同様の方法にて、融点275℃、相対粘度2.37の半芳香族ポリアミド(ポリアミド9N/M8N=50/50モル%)を得た(以下、この半芳香族ポリアミドを(B1-3)という。)。
半芳香族ポリアミド(B1-1)の製造において、1,9-ノナンジアミン2.374kg(15.0モル)と2-メチル-1,8-オクタンジアミン2.374kg(15.0モル)を1,10-デカンジアミン5.169kg(30.0モル)に変え、固相重合温度を230℃から260℃に変更した以外は、半芳香族ポリアミド(B1-1)の製造と同様の方法にて、融点315℃、相対粘度2.33の半芳香族ポリアミド(ポリアミド10T=100モル%)を得た(以下、この半芳香族ポリアミドを(B1-4)という。)。
半芳香族ポリアミド(B1-4)の製造において、1,10-デカンジアミン5.169kg(30.0モル)とテレフタル酸4.984kg(30.0モル)を1,10-デカンジアミン3.101kg(18.0モル)、テレフタル酸2.990kg(18.0モル)、及び11-アミノウンデカン酸2.416kg(12.0モル)に変え、固相重合温度を260℃から200℃に変更した以外は、半芳香族ポリアミド(B1-4)の製造と同様の方法にて、融点255℃、相対粘度2.34の半芳香族ポリアミド(ポリアミド10T/11=60/40モル%)を得た(以下、この半芳香族ポリアミドを(B1-5)という。)。
半芳香族ポリアミド(B1-4)の製造において、テレフタル酸4.984kg(30.0モル)をテレフタル酸3.324kg(20.0モル)とセバシン酸2.020kg(9.99モル)に変え、固相重合温度を260℃から220℃に変更した以外は、半芳香族ポリアミド(B1-4)の製造と同様の方法にて、融点279℃、相対粘度2.37の半芳香族ポリアミド(ポリアミド10T/1010=67/33モル%)を得た(以下、この半芳香族ポリアミドを(B1-6)という。)。
半芳香族ポリアミド(B1-4)の製造において、1,10-デカンジアミン5.169kg(30.0モル)とテレフタル酸4.984kg(30.0モル)を1,10-デカンジアミンとテレフタル酸の等モル塩7.258kg(24.0モル)、1,6-ヘキサンジアミンとドデカン二酸の等モル塩1.863kg(6.0)モルに変え、固相重合温度を260℃から210℃に変更した以外は、半芳香族ポリアミド(B1-4)の製造と同様の方法にて、融点261℃、相対粘度2.34の半芳香族ポリアミド(ポリアミド10T/612=80/20モル%)を得た(以下、この半芳香族ポリアミドを(B1-7)という。)。
半芳香族ポリアミド(B1-1)の製造において、固相重合時間を8時間から4時間に変更した以外は、半芳香族ポリアミド(B1-1)の製造と同様の方法にて、融点265℃、相対粘度2.08の半芳香族ポリアミド(ポリアミド9T/M8T=50/50モル%)を得た(以下、この半芳香族ポリアミドを(B1-8)という。)。
半芳香族ポリアミド(B1-1)の製造において、テレフタル酸4.939kg(29.7モル)、1,9-ノナンジアミン2.374kg(15.0モル)、及び2-メチル-1,8-オクタンジアミン2.374kg(15.0モル)をテレフタル酸2.741kg(16.5モル)、イソフタル酸0.997kg(6.0モル)、アジピン酸1.096kg(7.5モル)、及び1,6-ヘキサンジアミン3.602kg(31.0モル)に変え、重合温度を250℃、固相重合温度を230℃に変更した以外は、半芳香族ポリアミド(B1-1)の製造と同様の方法にて、融点302℃、相対粘度2.28の半芳香族ポリアミド(ポリアミド6T/6I/66=55/20/25モル%)を得た(以下、この半芳香族ポリアミドを(B1-9)という。)。
半芳香族ポリアミド(B2-1)の製造
攪拌機、温度計、トルクメータ、圧力計、ダイアフラムポンプを直結した原料投入口、窒素ガス導入口、放圧口、圧力調整装置、及びポリマー放出口を備えた内容積が70リットルの圧力容器に、セバシン酸6.068kg(30.0モル)、次亜リン酸カルシウム8.50g(0.049モル)、及び酢酸ナトリウム2.19g(0.025モル)を仕込み、圧力容器の内部の純度が99.9999%の窒素ガスで0.3MPaに加圧した後、次に常圧まで窒素ガスを放出する操作を5回繰返し、窒素置換を行った後、封圧下、攪拌しながら系内を昇温した。更に少量の窒素気流下で、190℃まで昇温した後、m-キシリレンジアミン4.086kg(30.0モル)を撹拌下で160分を要して滴下した。この間、反応系内圧は0.5MPaに制御し、内温を連続的に295℃まで昇温させた。また、m-キシリレンジアミンの滴下とともに留出する水は分縮器及び冷却器を通して系外に除いた。m-キシリレンジアミン滴下終了後、60分間かけて常圧まで降圧し、この間に、容器内の温度を250℃に保持して10分間反応を継続した。その後、反応系内圧を79kPaまで減圧し、40分間溶融重合反応を継続した。その後、攪拌を止めて系内を窒素で0.2MPaに加圧して重縮合物を圧力容器下部抜出口より紐状に抜き出した。紐状の重縮合物は直ちに冷却し、水冷した紐状の樹脂はペレタイザーによってペレット化し、その後、減圧乾燥を行い融点191℃、相対粘度2.46の半芳香族ポリアミド(ポリアミドMXD10=100モル%)を得た(以下、この半芳香族ポリアミドを(B2-1)という。)。
半芳香族ポリアミド(B2-1)の製造において、m-キシリレンジアミン4.086kg(30.0モル)をm-キシリレンジアミンとp-キシリレンジアミンの7:3の混合ジアミン4.086kg(30.0モル)に変え、重合温度を250℃から260℃に変更した以外は、半芳香族ポリアミド(B2-1)の製造と同様の方法にて、融点215℃、相対粘度2.40の半芳香族ポリアミド(ポリアミドMXD10/PXD10=70/30モル%)を得た(以下、この半芳香族ポリアミドを(B2-2)という。)。
半芳香族ポリアミド(B2-1)の製造において、m-キシリレンジアミン4.086kg(30.0モル)をm-キシリレンジアミンとp-キシリレンジアミンの6:4の混合ジアミン4.086kg(30.0モル)に変え、重合温度を250℃から270℃に変更した以外は、半芳香族ポリアミド(B2-1)の製造と同様の方法にて、融点224℃、相対粘度2.42の半芳香族ポリアミド(ポリアミドMXD10/PXD10=60/40モル%)を得た(以下、この半芳香族ポリアミドを(B2-3)という。)。
半芳香族ポリアミド(B2-1)の製造において、m-キシリレンジアミン4.086kg(30.0モル)をp-キシリレンジアミン4.086kg(30.0モル)に変え、重合温度を250℃から300℃に変更した以外は、半芳香族ポリアミド(B2-1)の製造と同様の方法にて、融点281、291℃(融点を2つ有する)、相対粘度2.42の半芳香族ポリアミド(ポリアミドPXD10=100モル%)を得た(以下、この半芳香族ポリアミドを(B2-4)という。)。
半芳香族ポリアミド(B2-1)の製造において、セバシン酸6.068kg(30.0モル)をアゼライン酸5.647kg(30.0モル)に変更した以外は、半芳香族ポリアミド(B2-1)の製造と同様の方法にて、融点194℃、相対粘度2.45の半芳香族ポリアミド(ポリアミドMXD9=100モル%)を得た(以下、この半芳香族ポリアミドを(B2-5)という。)。
半芳香族ポリアミド(B2-1)の製造において、m-キシリレンジアミン4.086kg(30.0モル)を2,6-ビス(アミノメチル)ナフタレン5.588kg(30.0モル)に変え、重合温度を240℃から300℃に変更した以外は、半芳香族ポリアミド(B2-1)の製造と同様の方法にて、融点286℃、相対粘度2.33の半芳香族ポリアミド(ポリアミド2,6-BAN10=100モル%)を得た(以下、この半芳香族ポリアミドを(B2-6)という。)。
半芳香族ポリアミド(B2-1)の製造において、溶融重合時間を40分から20分に変更した以外は、半芳香族ポリアミド(B2-1)の製造と同様の方法にて、融点191℃、相対粘度2.15の半芳香族ポリアミド(ポリアミドMXD10=100モル%)を得た(以下、この半芳香族ポリアミドを(B2-7)という。)。
半芳香族ポリアミド(B2-1)の製造において、セバシン酸6.068kg(30.0モル)をアジピン酸4.384kg(30.0モル)に変え、重合温度を250℃から275℃に変更した以外は、半芳香族ポリアミド(B2-1)の製造と同様の方法にて、融点243℃、相対粘度2.42の半芳香族ポリアミド(ポリアミドMXD6=100モル%)を得た(以下、この半芳香族ポリアミドを(B2-8)という。)。
半芳香族ポリアミド組成物(B-1)の製造
半芳香族ポリアミド(B1-1)に、衝撃改良材として無水マレイン酸変性エチレン/1-ブテン共重合体(A3-1)、酸化防止剤としてトリエチレングリコール-ビス[3-(3-t-ブチル-5-メチル-4-ヒドロキシフェニル)プロピオネート](BASFジャパン社製、IRGANOX245)、及びリン系加工安定剤としてトリス(2,4-ジ-t-ブチルフェニル)ホスファイト(BASFジャパン社製、IRGAFOS168)をあらかじめ混合し、二軸溶融混練機((株)日本製鋼所製、型式:TEX44)に供給し、シリンダ温度220℃から300℃で溶融混練し、溶融樹脂をストランド状に押出した後、これを水槽に導入し、冷却、カット、真空乾燥して、半芳香族ポリアミド(B1-1)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-1)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B1-2)に変え、シリンダ温度を300℃から340℃に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B1-2)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-2)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B1-3)に変え、シリンダ温度を300℃から310℃に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B1-3)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-3)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B1-4)に変え、シリンダ温度を300℃から340℃に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B1-4)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-4)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B1-5)に変え、シリンダ温度を300℃から290℃に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B1-5)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-5)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B1-6)に変え、シリンダ温度を300℃から310℃に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B1-6)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-6)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B1-7)に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B1-7)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-7)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B1-9)に変え、シリンダ温度を300℃から340℃に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B1-9)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-8)という。)。
半芳香族ポリアミド組成物(B-1)の製造において、半芳香族ポリアミド(B1-1)を(B2-1)に変え、シリンダ温度を300℃から240℃に変更した以外は、半芳香族ポリアミド組成物(B-1)の製造と同様の方法にて、半芳香族ポリアミド(B2-1)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-9)という。)。
半芳香族ポリアミド組成物(B-9)の製造において、半芳香族ポリアミド(B2-1)を(B2-2)に変え、シリンダ温度を240℃から250℃に変更した以外は、半芳香族ポリアミド組成物(B-9)の製造と同様の方法にて、半芳香族ポリアミド(B2-2)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-10)という。)。
半芳香族ポリアミド組成物(B-9)の製造において、半芳香族ポリアミド(B2-1)を(B2-3)に変え、シリンダ温度を240℃から260℃に変更した以外は、半芳香族ポリアミド組成物(B-9)の製造と同様の方法にて、半芳香族ポリアミド(B2-3)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-11)という。)。
半芳香族ポリアミド組成物(B-9)の製造において、半芳香族ポリアミド(B2-1)を(B2-4)に変え、シリンダ温度を240℃から320℃に変更した以外は、半芳香族ポリアミド組成物(B-9)の製造と同様の方法にて、半芳香族ポリアミド(B2-4)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-12)という。)。
半芳香族ポリアミド組成物(B-9)の製造において、半芳香族ポリアミド(B2-1)を(B2-5)に変更した以外は、半芳香族ポリアミド組成物(B-9)の製造と同様の方法にて、半芳香族ポリアミド(B2-5)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-13)という。)。
半芳香族ポリアミド組成物(B-9)の製造において、半芳香族ポリアミド(B2-1)を(B2-6)に変え、シリンダ温度を240℃から320℃に変更した以外は、半芳香族ポリアミド組成物(B-9)の製造と同様の方法にて、半芳香族ポリアミド(B2-6)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-14)という。)。
半芳香族ポリアミド組成物(B-9)の製造において、半芳香族ポリアミド(B2-1)を(B2-8)に変え、シリンダ温度を240℃から280℃に変更した以外は、半芳香族ポリアミド組成物(B-9)の製造と同様の方法にて、半芳香族ポリアミド(B2-8)90質量%、エラストマー重合体(A3-1)10質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる半芳香族ポリアミド組成物のペレットを得た(以下、この半芳香族ポリアミド組成物を(B-15)という。)。
半芳香族ポリアミド(B1-8)に、衝撃改良材として無水マレイン酸変性エチレン/1-ブテン共重合体(A3-1)とエチレン/1-ブテン共重合体(三井化学(株)製、タフマーA-0550)、導電性フィラーとしてカーボンブラック(ライオン(株)製、ケッチェンブラックEC600JD)、酸化防止剤としてトリエチレングリコール-ビス[3-(3-t-ブチル-5-メチル-4-ヒドロキシフェニル)プロピオネート](BASFジャパン社製、IRGANOX245)、及びリン系加工安定剤としてトリス(2,4-ジ-t-ブチルフェニル)ホスファイト(BASFジャパン社製、IRGAFOS168)をあらかじめ混合し、二軸溶融混練機((株)日本製鋼所製、型式:TEX44)に供給し、シリンダ温度240℃から320℃で溶融混練し、溶融樹脂をストランド状に押出した後、これを水槽に導入し、冷却、カット、真空乾燥して、半芳香族ポリアミド(B1-8)68質量%、エラストマー重合体(A3-1)を含む衝撃改良材25質量%、導電性フィラー7質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる導電性半芳香族ポリアミド組成物のペレットを得た(以下、この導電性半芳香族ポリアミド組成物を(B-16)という。)。
導電性半芳香族ポリアミド組成物(B-16)の製造において、半芳香族ポリアミド(B1-8)を(B2-7)に変え、シリンダ温度を320℃から270℃に変更した以外は、導電性半芳香族ポリアミド組成物(B-16)の製造と同様の方法にて、半芳香族ポリアミド(B2-7)68質量%、エラストマー重合体(A3-1)を含む衝撃改良材25質量%、導電性フィラー7質量%の合計100質量部に対して、酸化防止剤0.8質量部、リン系加工安定剤0.2質量部よりなる導電性半芳香族ポリアミド組成物のペレットを得た(以下、この導電性半芳香族ポリアミド組成物を(B-17)という。)。
含フッ素系重合体(C-1)の製造
内容積が100Lの撹拌機付き重合槽を脱気し、1-ヒドロトリデカフルオロヘキサンの92.1kg、1,3-ジクロロ-1,1,2,2,3-ペンタフルオロプロパン16.3kg、(パーフルオロエチル)エチレンCH2=CH(CF2)2F73g、無水イタコン酸(IAH)10.1gを仕込み、テトラフルオロエチレン(TFE)9.6kg、エチレン(E)0.7kgを圧入し、重合槽内を66℃に昇温し、重合開始剤としてt-ブチルペルオキシピバレート1質量%1,3-ジクロロ-1,1,2,2,3-ペンタフルオロプロパン溶液の433cm3を仕込み、重合を開始させた。重合中圧力が一定になるようにTFE/E:60/40(モル比)のモノマー混合ガスを連続的に仕込んだ。また、重合中に仕込むTFEとEの合計モル数に対して2.0モル%に相当する量の(パーフルオロエチル)エチレンと0.5モル%に相当する量のIAHを連続的に仕込んだ。重合開始5.5時間後、モノマー混合ガス8.0kg、IAHの63gを仕込んだ時点で、重合槽内温を室温まで降温し、パージして圧力を常圧とした。得られたスラリ状の含フッ素系重合体を、水75.0kgを仕込んだ200Lの造粒槽に投入し、次いで撹拌しながら105℃まで昇温し溶媒を留出除去しながら造粒した。得られた造粒物を150℃で5時間乾燥することにより、8.3kgの含フッ素系重合体が得られた。
当該含フッ素系重合体の組成は、TFEに基づく重合単位/Eに基づく重合単位/CH2=CH(CF2)2Fに基づく重合単位/IAHに基づく重合単位=58.5/39.0/2.0/0.5(モル%)であり、融点は240℃であった。この造粒物を、押出機を用いて、280℃、滞留時間2分で溶融し、含フッ素系重合体のペレットを得た(以下、この含フッ素系重合体を(C-1)という。)。
含フッ素系重合体(C-1)100質量部、及びカーボンブラック(電気化学(株)製)13質量部をあらかじめ混合し、二軸溶融混練機(東芝機械(株)製、型式:TEM-48S)に供給し、シリンダ温度240℃から300℃で溶融混練し、溶融樹脂をストランド状に押出した後、これを水槽に導入し、吐出したストランドを水冷し、ペレタイザーでストランドを切断し、水分除去のために120℃の乾燥機で10時間乾燥し、導電性含フッ素系重合体組成物のペレットを得た(以下、この導電性含フッ素系重合体組成物を(C-2)という。)。
含フッ素系重合体(C-1)の製造において、無水イタコン酸(IAH)を仕込まない以外は、含フッ素系重合体(C-1)の製造と同様の方法にて、7.6kgの含フッ素系重合体を得た。
当該含フッ素系重合体の組成は、TFEに基づく重合単位/Eに基づく重合単位/CH2=CH(CF2)2Fに基づく重合単位/IAHに基づく重合単位=58.8/39.2/2.0(モル%)であり、融点は242℃であった。この造粒物を、押出機を用いて、280℃、滞留時間2分で溶融し、含フッ素系重合体のペレットを得た(以下、この含フッ素系重合体を(C-3)という。)。
導電性含フッ素系重合体組成物(C-2)の製造において、含フッ素系重合体(C-1)を(C-3)に変更した以外は、導電性含フッ素系重合体組成物(C-2)の製造と同様の方法にて、導電性含フッ素系重合体組成物のペレットを得た(以下、この導電性含フッ素系重合体組成物を(C-4)という。)。
内容積が100Lの撹拌機付き重合槽を脱気し、1,3-ジクロロ-1,1,2,2,3-ペンタフルオロプロパン42.5kg、CF2=CFOCF2CF2CF3(パーフルオロ(プロピルビニルエーテル):PPVE)、1,1,2,4,4,5,5,6,6,6-デカフルオロ-3-オキサヘックス-1-エン)2.13kg、ヘキサフルオロプロピレン(HFP)51.0kgを仕込んだ。ついで重合槽内を50℃に昇温し、テトラフルオロエチレン(TFE)の4.25kgを仕込んで圧力を1.0MPa/Gまで昇圧した。重合開始剤溶液として(ペルフルオロブチリル)ペルオキシド0.3質量%1,3-ジクロロ-1,1,2,2,3-ペンタフルオロプロパン溶液の340cm3を仕込み、重合を開始させ、以後10分毎に当該重合開始剤溶液の340cm3を仕込んだ。重合中、圧力が1.0MPa/Gを保持するようにTFEを連続的に仕込んだ。また、重合中に仕込むTFEのモル数に対して0.1モル%に相当する量の5-ノルボルネン-2,3-ジカルボン酸無水物(NAH)0.3質量%1,3-ジクロロ-1,1,2,2,3-ペンタフルオロプロパン溶液を連続的に仕込んだ。重合開始5時間後、TFE8.5kgを仕込んだ時点で、重合槽内温を室温まで降温するとともに常圧までパージした。得られたスラリ状の含フッ素系重合体を、水75.0kgを仕込んだ200Lの造粒槽に投入し、次いで撹拌しながら105℃まで昇温し溶媒を留出除去しながら造粒した。得られた造粒物を150℃で5時間乾燥することにより、7.5kgの含フッ素系重合体の造粒物が得られた。
含フッ素系重合体(C-5)の製造において、5-ノルボルネン-2,3-ジカルボン酸無水物(NAH)0.3質量%1,3-ジクロロ-1,1,2,2,3-ペンタフルオロプロパン溶液を仕込まない以外は、含フッ素系重合体(C-5)の製造と同様の方法にて、7.6kgの含フッ素系重合体を得た。
当該含フッ素系重合体の組成は、TFEに基づく重合単位/PPVEに基づく重合単位/HFPに基づく重合単位=91.5/1.5/7.0(モル%)であり、融点は257℃であった。この造粒物を、押出機を用いて、300℃、滞留時間2分で溶融し、含フッ素系重合体のペレットを得た(以下、この含フッ素系重合体を(C-6)という。)。
導電性含フッ素系重合体組成物(C-2)の製造において、含フッ素系重合体(C-1)を(C-6)、カーボンブラック13質量部を11質量部に変え、シリンダ温度を300℃から320℃に変更した以外は、導電性含フッ素系重合体組成物(C-2)の製造と同様の方法にて、導電性含フッ素系重合体組成物のペレットを得た(以下、この導電性含フッ素系重合体組成物を(C-7)という。)。
水174kgを収容できるジャケット付攪拌式重合槽に、脱ミネラルした純水 51.5kgを仕込み、内部空間を純窒素ガスで充分置換した後、窒素ガスを真空で排除した。次いでオクタフルオロシクロブタン40.6kg、クロロトリフルオロエチレン(CTFE)1.6kg、テトラフルオロエチレン(TFE)4.5kg、パーフルオロ(プロピルビニルエーテル)(PPVE)2.8kgを圧入した。連鎖移動剤としてn-プロピルアルコール0.090kgを添加して、温度を35℃に調節し、攪拌を開始した。ここへ重合開始剤としてジ-n-プロピルパーオキシジカーボネート50質量%メタノール溶液を0.44kg添加して重合を開始した。重合中には、所望の共重合体組成と同組成に調製した混合モノマーを、槽内圧力が0.66MPaを維持するように追加仕込みしながら重合した後、槽内の残存ガスを排気して生成したポリマーを取り出し、脱ミネラルした純水で洗浄し、乾燥させて30.5kgの粒状粉末の含フッ素系重合体を得た。
当該フッ素系重合体の組成は、CTFEに基づく重合単位/TFEに基づく重合単位/PPVEに基づく重合単位のモル比で24.4/73.1/2.5であり、含フッ素系重合体中の主鎖炭素原子数1×106個に対するカーボネート末端基の数は170個であった。また、融点は241℃であった。この造粒物を、押出機を用いて、290℃、滞留時間2分で溶融し、含フッ素系重合体のペレットを得た(以下、この含フッ素系重合体を(C-8)という。)。
含フッ素系重合体(C-8)の製造において、ジ-n-プロピルパーオキシジカーボネート50質量%メタノール溶液を仕込まない以外は、含フッ素系重合体(C-9)の製造と同様の方法にて、29.8kgの含フッ素系重合体を得た。
当該含フッ素系重合体の組成は、CTFEに基づく重合単位/TFEに基づく重合単位/PPVEに基づく重合単位のモル比で24.4/73.1/2.5であり、融点は241℃であった。この造粒物を、押出機を用いて、290℃、滞留時間2分で溶融し、含フッ素系重合体のペレットを得た(以下、この含フッ素系重合体を(C-9)という。)。
導電性含フッ素系重合体組成物(C-7)の製造において、含フッ素系重合体(C-6)を(C-9)に変え、シリンダ温度を320℃から300℃に変更した以外は、導電性含フッ素系重合体組成物(C-7)の製造と同様の方法にて、導電性含フッ素系重合体組成物のペレットを得た(以下、この導電性含フッ素系重合体組成物を(C-10)という。)。
前記に示すポリアミド12組成物(A-1)、半芳香族ポリアミド組成物(B-1)を使用して、Plabor(プラスチック工学研究所(株)製)2層チューブ成形機にて、(A-1)を押出温度270℃、(B-1)を押出温度300℃にて別々に溶融させ、吐出された溶融樹脂をアダプタによって合流させ、積層管状体に成形した。引き続き、寸法制御するサイジングダイにより冷却し、引き取りを行い、(A-1)からなる(a)層(最外層)、(B-1)からなる(b)層(最内層)としたとき、層構成が(a)/(b)=0.75/0.25mmで内径6mm、外径8mmの積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-2)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-3)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-4)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-5)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-6)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-7)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)をポリアミド1010組成物(A-8)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-2)に変え、(B-2)の押出温度を340℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-3)に変え、(B-3)の押出温度を310℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-4)に変え、(B-4)の押出温度を340℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-5)に変え、(B-5)の押出温度を290℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-6)に変え、(B-6)の押出温度を310℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-7)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-9)に変え、(B-9)の押出温度を240℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-10)に変え、(B-10)の押出温度を250℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-11)に変え、(B-11)の押出温度を260℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-12)に変え、(B-12)の押出温度を320℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-13)に変え、(B-13)の押出温度を240℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-14)に変え、(B-14)の押出温度を320℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を導電性半芳香族ポリアミド組成物(B-16)に変え、(B-16)の押出温度を320℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
実施例1において、半芳香族ポリアミド組成物(B-1)を導電性半芳香族ポリアミド組成物(B-17)に変え、(B-17)の押出温度を270℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
前記に示すポリアミド12組成物(A-1)、半芳香族ポリアミド組成物(B-1)、導電性半芳香族ポリアミド組成物(B-16)を使用して、Plabor(プラスチック工学研究所(株)製)3層チューブ成形機にて、(A-1)を押出温度270℃、(B-1)を押出温度300℃、(B-16)を押出温度320℃にて別々に溶融させにて、吐出された溶融樹脂をアダプタによって合流させ、積層管状体に成形した。引き続き、寸法制御するサイジングダイにより冷却し、引き取りを行い、(A-1)からなる(a)層(最外層)、(B-1)からなる(b)層(中間層)、(B-16)からなる(b’)層(最内層)としたとき、層構成が(a)/(b)/(b’)=0.75/0.15/0.10mmで内径6mm、外径8mmの積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
実施例23において、半芳香族ポリアミド組成物(B-1)を(B-9)、導電性半芳香族ポリアミド組成物(B-16)を(B-17)に変え、(B-9)の押出温度を240℃、(B-17)の押出温度を270℃に変更した以外は、実施例23と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
前記に示すポリアミド12組成物(A-1)、半芳香族ポリアミド組成物(B-1)、含フッ素系重合体(C-1)を使用して、Plabor(プラスチック工学研究所(株)製)3層チューブ成形機にて、(A-1)を押出温度270℃、(B-1)を押出温度300℃、(C-1)を押出温度290℃にて別々に溶融させ、吐出された溶融樹脂をアダプタによって合流させ、管状に成形し、寸法制御するサイジングダイにより冷却し、引き取りを行い、(A-1)からなる層を(a)層(最外層)、(B-1)からなる層を(b)層(中間層)、(C-1)からなる層を(c)層(最内層)としたとき、層構成が(a)/(b)/(c)=0.70/0.15/0.15mm、内径6mm、外径8mmの積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例25において、半芳香族ポリアミド組成物(B-1)を(B-9)に変え、(B-9)の押出温度を240℃に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。当該積層チューブの物性測定結果を表1に示す。
実施例25において、含フッ素系重合体(C-1)を導電性含フッ素系重合体(C-2)に変え、(C-2)の押出温度を310℃に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
実施例25において、含フッ素系重合体(C-1)を(C-5)に変え、(C-5)の押出温度を310℃に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。当該積層チューブの物性測定結果を表1に示す。
実施例25において、含フッ素系重合体(C-1)を(C-8)に変え、(C-8)の押出温度を300℃に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。当該積層チューブの物性測定結果を表1に示す。
前記に示すポリアミド12組成物(A-1)、半芳香族ポリアミド組成物(B-1)、含フッ素系重合体(C-1)、導電性含フッ素系重合体(C-2)を使用して、Plabor(プラスチック工学研究所(株)製)4層チューブ成形機にて、(A-1)を押出温度270℃、(B-1)を押出温度300℃、(C-1)を押出温度290℃、(C-2)を押出温度310℃にて別々に溶融させ、吐出された溶融樹脂をアダプタによって合流させ、管状に成形し、寸法制御するサイジングダイにより冷却し、引き取りを行い、(A-1)からなる層を(a)層(最外層)、(B-1)からなる層を(b)層(中間層)、(C-1)からなる層を(c)層(内層)、(C-2)からなる層を(c’)層(最内層)としたとき、層構成が(a)/(b)/(c)/(c’)=0.65/0.15/0.10/0.10mm、内径6mm、外径8mmの積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
実施例30において、半芳香族ポリアミド組成物(B-1)を(B-9)に変え、(B-9)の押出温度を240℃に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。当該積層チューブの物性測定結果を表1に示す。
実施例30において、導電性含フッ素系重合体(C-2)を含フッ素系重合体(C-3)に変え、(C-3)の押出温度を290℃に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、導電性含フッ素系重合体(C-2)を(C-4)に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
実施例30において、含フッ素系重合体(C-1)を(C-5)、導電性含フッ素系重合体(C-2)を含フッ素系重合体(C-6)に変え、(C-5)の押出温度を310℃に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、含フッ素系重合体(C-1)を(C-5)、導電性含フッ素系重合体(C-2)を(C-7)に変え、(C-5)の押出温度を310℃、(C-7)の押出温度を330℃に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
実施例30において、含フッ素系重合体(C-1)を(C-8)、導電性含フッ素系重合体(C-2)を含フッ素系重合体(C-9)に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、含フッ素系重合体(C-1)を(C-8)、導電性含フッ素系重合体(C-2)を(C-10)に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。また、当該積層チューブの導電性をSAE J-2260に準拠して測定したところ、106Ω/square以下であり、静電気除去性能に優れていることを確認した。
実施例1において、ポリアミド12組成物(A-1)を(A-9)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-10)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-11)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、ポリアミド12組成物(A-1)を(A-12)に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-8)に変え、(B-8)の押出温度を350℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例1において、半芳香族ポリアミド組成物(B-1)を(B-15)に変え、(B-15)の押出温度を280℃に変更した以外は、実施例1と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例25において、ポリアミド12組成物(A-1)を(A-9)に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例25において、ポリアミド12組成物(A-1)を(A-10)に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例25において、ポリアミド12組成物(A-1)を(A-11)に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例25において、ポリアミド12組成物(A-1)を(A-12)に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例25において、半芳香族ポリアミド組成物(B-1)を(B-8)に変え、(B-8)の押出温度を350℃に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例25において、半芳香族ポリアミド組成物(B-1)を(B-15)に変え、(B-15)の押出温度を280℃に変更した以外は、実施例25と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、ポリアミド12組成物(A-1)を(A-9)に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、ポリアミド12組成物(A-1)を(A-10)に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、ポリアミド12組成物(A-1)を(A-11)に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、ポリアミド12組成物(A-1)を(A-12)に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、半芳香族ポリアミド組成物(B-1)を(B-8)に変え、(B-8)の押出温度を350℃に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
実施例30において、半芳香族ポリアミド組成物(B-1)を(B-15)に変え、(B-15)の押出温度を280℃に変更した以外は、実施例30と同様の方法にて、表1に示す層構成の積層チューブを得た。当該積層チューブの物性測定結果を表1に示す。
一方、本発明に規定されている実施例1から37の積層チューブは、耐薬品性、層間接着性、及びその耐久性等の諸特性が良好であることは明らかである。
Claims (11)
- (a)層と(b)層とを含む2層以上の積層チューブであって、
少なくとも1組の前記(a)層と前記(b)層とは、隣接して配置され、
前記(a)層は、脂肪族ポリアミド組成物(A)を含み、
前記(b)層は、半芳香族ポリアミド組成物(B)を含み、
前記脂肪族ポリアミド組成物(A)は、ポリアミド(A1)、ポリアミド(A2)、及びエラストマー重合体(A3)を含み、
前記ポリアミド(A1)は、メチレン基数のアミド基数に対する比が8.0以上の脂肪族ポリアミドであり、前記脂肪族ポリアミド組成物(A)中に、40質量%以上90質量%以下含まれ、
前記ポリアミド(A2)は、前記ポリアミド(A1)以外のポリアミドであり、前記脂肪族ポリアミド組成物(A)中に、5質量%以上30質量%以下含まれ、
前記エラストマー重合体(A3)は、カルボキシル基及び/又は酸無水物基を有する不飽和化合物から誘導される構成単位を含有し、前記脂肪族ポリアミド組成物(A)中に、5質量%以上30質量%以下含まれ、
前記ポリアミド(A1)と前記ポリアミド(A2)との溶解性パラメーターSP値の差の絶対値[|(ポリアミド(A1)のSP値)-(ポリアミド(A2)のSP値)|]は1.8以上5.5以下(MPa)1/2であり、
前記半芳香族ポリアミド組成物(B)は、半芳香族ポリアミド(B1)又は半芳香族ポリアミド(B2)を含み、
前記半芳香族ポリアミド組成物(B)中に、前記半芳香族ポリアミド(B1)又は前記半芳香族ポリアミド(B2)が60質量%以上含まれ、
前記半芳香族ポリアミド(B1)は、前記半芳香族ポリアミド(B1)の全ジアミン単位に対して、炭素原子数9又は10の脂肪族ジアミン単位を50モル%以上含み、前記半芳香族ポリアミド(B1)の全ジカルボン酸単位に対して、テレフタル酸単位及び/又ナフタレンジカルボン酸単位を50モル%以上含み、
前記半芳香族ポリアミド(B2)は、前記半芳香族ポリアミド(B2)の全ジアミン単位に対して、キシリレンジアミン単位及び/又はビス(アミノメチル)ナフタレン単位を50モル%以上含み、前記半芳香族ポリアミド(B2)の全ジカルボン酸単位に対して、炭素原子数9又は10の脂肪族ジカルボン酸単位を50モル%以上含む積層チューブ。 - 前記ポリアミド(A1)が、ポリヘキサメチレンドデカミド(ポリアミド612)、ポリノナメチレンドデカミド(ポリアミド912)、ポリデカメチレンセバカミド(ポリアミド1010)、ポリデカメチレンドデカミド(ポリアミド1012)、ポリドデカメチレンドデカミド(ポリアミド1212)、ポリウンデカンアミド(ポリアミド11)、及びポリドデカンアミド(ポリアミド12)からなる群より選ばれる少なくとも1種の単独重合体、並びに/又はこれらを形成する原料単量体を数種用いた共重合体である請求項1に記載の積層チューブ。
- 前記ポリアミド(A2)が、ポリカプロアミド(ポリアミド6)、ポリヘキサメチレンアジパミド(ポリアミド66)、ポリヘキサメチレンアゼラミド(ポリアミド69)、ポリヘキサメチレンセバカミド(ポリアミド610)、ポリヘキサメチレンテレフタラミド(ポリアミド6T)、ポリヘキサメチレンイソフタラミド(ポリアミド6I)、及びポリメタキシリレンアジパミド(ポリアミドMXD6)からなる群より選ばれる少なくとも1種の単独重合体、並びに/若しくはこれらを形成する原料単量体を数種用いた共重合体、又は、前記ポリカプロアミド(ポリアミド6)、ポリヘキサメチレンアジパミド(ポリアミド66)、ポリヘキサメチレンアゼラミド(ポリアミド69)、ポリヘキサメチレンセバカミド(ポリアミド610)、ポリヘキサメチレンテレフタラミド(ポリアミド6T)、ポリヘキサメチレンイソフタラミド(ポリアミド6I)、及びポリメタキシリレンアジパミド(ポリアミドMXD6)からなる群より選ばれる少なくとも1種を形成する原料単量体を主成分とし、ポリヘキサメチレンドデカミド(ポリアミド612)、ポリノナメチレンドデカミド(ポリアミド912)、ポリデカメチレンセバカミド(ポリアミド1010)、ポリデカメチレンドデカミド(ポリアミド1012)、ポリドデカメチレンドデカミド(ポリアミド1212)、ポリウンデカンアミド(ポリアミド11)、及びポリドデカンアミド(ポリアミド12)からなる群より選ばれる少なくとも1種を形成する原料単量体を数種用いた共重合体である請求項1又は2のいずれか1項に記載の積層チューブ。
- 前記脂肪族ポリアミド組成物(A)中の前記ポリアミド(A1)及び前記ポリアミド(A2)それぞれにおける1gあたりの末端アミノ基濃度を[A](μeq/g)、末端カルボキシル基濃度を[B](μeq/g)とした時、[A]>[B]+10である請求項1から3のいずれか1項に記載の積層チューブ。
- 前記半芳香族ポリアミド組成物(B)が、前記エラストマー重合体(A3)を含む請求項1から4のいずれか1項に記載の積層チューブ。
- 前記(b)層が、前記(a)層に対して内側に隣接して配置される請求項1から5のいずれか1項に記載の積層チューブ。
- 更に(c)層を含み、
少なくとも1組の前記(b)層と前記(c)層とが隣接して配置され、
前記(c)層は、アミノ基に対して反応性を有する官能基が分子鎖中に導入された含フッ素系重合体(C)を含む請求項1から6のいずれか1項に記載の積層チューブ。 - 前記(c)層が、前記(b)層に対して内側に配置される請求項7に記載の積層チューブ。
- 最内層が、導電性フィラーを含有させた熱可塑性樹脂組成物を含む導電層である請求項1から8のいずれか1項に記載の積層チューブ。
- 共押出成形により製造される請求項1から9のいずれか1項に記載の積層チューブ。
- 燃料チューブとして使用される請求項1から10のいずれか1項に記載の積層チューブ。
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Publication number | Publication date |
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CN109311259B (zh) | 2021-05-25 |
KR102354735B1 (ko) | 2022-01-25 |
JP2022062055A (ja) | 2022-04-19 |
EP3437850A4 (en) | 2019-11-06 |
JP7010210B2 (ja) | 2022-01-26 |
BR112018069437B1 (pt) | 2022-09-06 |
JP7322983B2 (ja) | 2023-08-08 |
EP3437850A1 (en) | 2019-02-06 |
US11529787B2 (en) | 2022-12-20 |
EP3437850B1 (en) | 2021-05-12 |
BR112018069437A2 (pt) | 2019-02-12 |
CN109311259A (zh) | 2019-02-05 |
BR112018069437B8 (pt) | 2023-05-16 |
KR20180129866A (ko) | 2018-12-05 |
JPWO2017170985A1 (ja) | 2019-03-22 |
US20190091962A1 (en) | 2019-03-28 |
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