JP6996666B2 - ポリアミド樹脂組成物の製造方法 - Google Patents
ポリアミド樹脂組成物の製造方法 Download PDFInfo
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- JP6996666B2 JP6996666B2 JP2021541503A JP2021541503A JP6996666B2 JP 6996666 B2 JP6996666 B2 JP 6996666B2 JP 2021541503 A JP2021541503 A JP 2021541503A JP 2021541503 A JP2021541503 A JP 2021541503A JP 6996666 B2 JP6996666 B2 JP 6996666B2
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- polyamide resin
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- 229920006122 polyamide resin Polymers 0.000 title claims description 41
- 239000011342 resin composition Substances 0.000 title claims description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 238000000034 method Methods 0.000 title claims description 15
- 229920005989 resin Polymers 0.000 claims description 40
- 239000011347 resin Substances 0.000 claims description 40
- 239000012779 reinforcing material Substances 0.000 claims description 36
- 239000005749 Copper compound Substances 0.000 claims description 29
- 150000001880 copper compounds Chemical class 0.000 claims description 29
- 239000006229 carbon black Substances 0.000 claims description 17
- 239000003365 glass fiber Substances 0.000 claims description 17
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 12
- 229920006039 crystalline polyamide Polymers 0.000 claims description 12
- 239000000155 melt Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 229920006134 semi-aromatic non-crystalline polyamide resin Polymers 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000000113 differential scanning calorimetry Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- -1 polytetramethylene Polymers 0.000 description 23
- 238000012360 testing method Methods 0.000 description 20
- QTMDXZNDVAMKGV-UHFFFAOYSA-L copper(ii) bromide Chemical compound [Cu+2].[Br-].[Br-] QTMDXZNDVAMKGV-UHFFFAOYSA-L 0.000 description 12
- 238000000465 moulding Methods 0.000 description 9
- 239000004952 Polyamide Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229920002647 polyamide Polymers 0.000 description 8
- 239000000835 fiber Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 229910021590 Copper(II) bromide Inorganic materials 0.000 description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000010445 mica Substances 0.000 description 6
- 229910052618 mica group Inorganic materials 0.000 description 6
- GVNWZKBFMFUVNX-UHFFFAOYSA-N Adipamide Chemical compound NC(=O)CCCCC(N)=O GVNWZKBFMFUVNX-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000004898 kneading Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000002612 dispersion medium Substances 0.000 description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000008188 pellet Substances 0.000 description 4
- 229920006111 poly(hexamethylene terephthalamide) Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 4
- 229910021589 Copper(I) bromide Inorganic materials 0.000 description 3
- 229920002302 Nylon 6,6 Polymers 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000001361 adipic acid Substances 0.000 description 3
- 235000011037 adipic acid Nutrition 0.000 description 3
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 description 3
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 150000004985 diamines Chemical class 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 239000000454 talc Substances 0.000 description 3
- 229910052623 talc Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229920000299 Nylon 12 Polymers 0.000 description 2
- 229920002292 Nylon 6 Polymers 0.000 description 2
- 229920000305 Nylon 6,10 Polymers 0.000 description 2
- 229920006127 amorphous resin Polymers 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- YEOCHZFPBYUXMC-UHFFFAOYSA-L copper benzoate Chemical compound [Cu+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 YEOCHZFPBYUXMC-UHFFFAOYSA-L 0.000 description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
- ILRSCQWREDREME-UHFFFAOYSA-N dodecanamide Chemical compound CCCCCCCCCCCC(N)=O ILRSCQWREDREME-UHFFFAOYSA-N 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920006128 poly(nonamethylene terephthalamide) Polymers 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- GUOSQNAUYHMCRU-UHFFFAOYSA-N 11-Aminoundecanoic acid Chemical compound NCCCCCCCCCCC(O)=O GUOSQNAUYHMCRU-UHFFFAOYSA-N 0.000 description 1
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical compound NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 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 1
- JXSRRBVHLUJJFC-UHFFFAOYSA-N 7-amino-2-methylsulfanyl-[1,2,4]triazolo[1,5-a]pyrimidine-6-carbonitrile Chemical compound N1=CC(C#N)=C(N)N2N=C(SC)N=C21 JXSRRBVHLUJJFC-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229920000571 Nylon 11 Polymers 0.000 description 1
- 229920003189 Nylon 4,6 Polymers 0.000 description 1
- 229920000572 Nylon 6/12 Polymers 0.000 description 1
- 229920006152 PA1010 Polymers 0.000 description 1
- 229920006154 PA11T Polymers 0.000 description 1
- 229920006153 PA4T Polymers 0.000 description 1
- 229920006121 Polyxylylene adipamide Polymers 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 1
- HVYLDJKDVOOTHV-UHFFFAOYSA-N acetic acid;2-iminoethanethiol Chemical compound CC(O)=O.CC(O)=O.SCC=N HVYLDJKDVOOTHV-UHFFFAOYSA-N 0.000 description 1
- 229920001893 acrylonitrile styrene Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- KCLGATRJYMEERW-UHFFFAOYSA-N benzene-1,3-dicarboxylic acid;copper Chemical compound [Cu].OC(=O)C1=CC=CC(C(O)=O)=C1 KCLGATRJYMEERW-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- CMRVDFLZXRTMTH-UHFFFAOYSA-L copper;2-carboxyphenolate Chemical compound [Cu+2].OC1=CC=CC=C1C([O-])=O.OC1=CC=CC=C1C([O-])=O CMRVDFLZXRTMTH-UHFFFAOYSA-L 0.000 description 1
- ZCXLQZOQWCXFNN-UHFFFAOYSA-N copper;hexanedioic acid Chemical compound [Cu].OC(=O)CCCCC(O)=O ZCXLQZOQWCXFNN-UHFFFAOYSA-N 0.000 description 1
- LZJJVTQGPPWQFS-UHFFFAOYSA-L copper;propanoate Chemical compound [Cu+2].CCC([O-])=O.CCC([O-])=O LZJJVTQGPPWQFS-UHFFFAOYSA-L 0.000 description 1
- KTMJZMQYZGNYBQ-UHFFFAOYSA-L copper;pyridine-3-carboxylate Chemical compound [Cu+2].[O-]C(=O)C1=CC=CN=C1.[O-]C(=O)C1=CC=CN=C1 KTMJZMQYZGNYBQ-UHFFFAOYSA-L 0.000 description 1
- ZISLUDLMVNEAHK-UHFFFAOYSA-L copper;terephthalate Chemical compound [Cu+2].[O-]C(=O)C1=CC=C(C([O-])=O)C=C1 ZISLUDLMVNEAHK-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003484 crystal nucleating agent Substances 0.000 description 1
- 229940045803 cuprous chloride Drugs 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000052 poly(p-xylylene) Polymers 0.000 description 1
- 229920006396 polyamide 1012 Polymers 0.000 description 1
- 229920006394 polyamide 410 Polymers 0.000 description 1
- 229920006123 polyhexamethylene isophthalamide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- 239000006235 reinforcing carbon black Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229920006012 semi-aromatic polyamide Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- BPILDHPJSYVNAF-UHFFFAOYSA-M sodium;diiodomethanesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C(I)I BPILDHPJSYVNAF-UHFFFAOYSA-M 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- KLNPWTHGTVSSEU-UHFFFAOYSA-N undecane-1,11-diamine Chemical compound NCCCCCCCCCCCN KLNPWTHGTVSSEU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- 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
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/46—Post-polymerisation treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/105—Compounds containing metals of Groups 1 to 3 or of Groups 11 to 13 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
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- C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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- C08J2425/08—Copolymers of styrene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Description
また、半芳香族ポリアミド樹脂(MXD-6)にナイロン66、ガラス繊維、マイカを高充填し、強度・剛性を上げる方法(例えば、特許文献5)が知られているが、この場合、成形時の金型温度を135℃もの高温に上げる必要があり、高温に上げた場合でも良好な成形品外観が得られない場合もあった。
[1] (A)ポリカプラミド樹脂を主成分とする結晶性ポリアミド樹脂、(B)半芳香族非晶性ポリアミド樹脂、(C)無機強化材、(D)カーボンブラックのマスターバッチ、及び(E)銅化合物を含有するポリアミド樹脂組成物の製造方法であって、
該ポリアミド樹脂組成物は、
(C)無機強化材として、(C-1)ガラス繊維、(C-2)針状ワラストナイト、及び(C-3)板状晶の無機強化材を含み、
ポリアミド樹脂組成物の水分率0.05%以下でのメルトマスフローレイト(MFR)が4.0g/10分以上、13.0g/10分未満であり、
ポリアミド樹脂組成物の示差走査熱量計(DSC)で測定した降温結晶化温度(TC2)が、180℃以上、185℃以下であり、
(A)と(B)との質量比が0.5<(B)/(A)≦0.8を満足し、
(A)、(B)、(C)、及び(D)の合計を100質量部としたとき、(E)の含有量が、0.001~0.1質量部であり、各成分の含有量が下記式を満足し、
30質量部≦(A)+(B)+(D)≦60質量部
13質量部≦(B)≦23質量部
1質量部≦(D)≦5質量部
20質量部≦(C-1)≦40質量部
8質量部≦(C-2)≦25質量部
8質量部≦(C-3)≦25質量部
40質量部≦(C-1)+(C-2)+(C-3)≦70質量部
(E)銅化合物は、濃度を0.04質量%~1.0質量%とした分散液とし、
(A)ポリカプラミド樹脂を主成分とする結晶性ポリアミド樹脂、(B)半芳香族非晶性ポリアミド樹脂、(D)カーボンブラックのマスターバッチ、及び(E)銅化合物の分散液を予め混合して押出機のホッパー部に投入し、(C)無機強化材を押出機にサイドフィード方式によって投入することを特徴とするポリアミド樹脂組成物の製造方法。
[2] 前記(E)銅化合物の分散液が、(E)銅化合物の水溶液である[1]に記載のポリアミド樹脂組成物の製造方法。
本発明において、ポリアミド樹脂の結晶性/非晶性は、ポリアミド樹脂をJIS K 7121:2012に準じて昇温速度20℃/分でDSC測定した場合に、明確な融点ピークを示すものを結晶性、示さないものを非晶性とする。
本発明のポリアミド樹脂組成物中の各成分の含有量(配合量)は、特に但し書きをしない限り、(A)ポリカプラミド樹脂を主成分とする結晶性ポリアミド樹脂、(B)半芳香族非晶性ポリアミド樹脂、(C)無機強化材、及び(D)カーボンブラックのマスターバッチの合計を100質量部としたときの量で表している。
半芳香族非晶性ポリアミド樹脂の相対粘度(96%硫酸法)は、特に限定されるものではないが、好ましい範囲は1.8~2.4である。
0.5<(B)/(A)≦0.8
本発明において、(B)/(A)がこの範囲にあることで、より高いレベルの良好な外観の成形品が得られ、(B)/(A)は、0.52以上、0.75以下が好ましく、0.55以上、0.75以下がより好ましい。
(C)成分は、いずれもポリアミド樹脂組成物中で補強効果を発揮するが、その中でも(C-1)ガラス繊維が一番補強効果として高いが、成形品のソリ変形も大きい。(C-2)針状ワラストナイト、(C-3)板状晶の無機強化材は、ガラス繊維ほどの補強効果は無いものの、アスペクト比がガラス繊維よりも小さいため、ソリ変形が小さくなる利点がある。また、針状ワラストナイトは成形後のヒケ防止にも寄与でき、これらを適切に組み合わせることで、強化材が高濃度に配合されていても、成形後に大きな変形を生み出さない樹脂組成物を作製できる。
通常、ガラス繊維、ワラストナイトなどを高濃度に配合した強化ポリアミド樹脂組成物は、耐候性に劣り強化材の露出が発生するが、後述のカーボンブラックマスターバッチと銅化合物と組み合わせることにより耐候性を制御でき、強化材の露出を防ぐことが可能となる。
4)曲げ弾性率:JIS K 7171:2016に準じて測定した。
光沢度の測定結果を、「光沢度95以上:○、光沢度95未満~90以上:△、光沢度90未満:×」として表記した。
○:強化材の露出が認められない。×:強化材の露出が認められる。
8)耐候試験後の成形品表面のシボ状態:上記6)の耐候試験後のシボ平板について、目視にて、下記の指標で判断した。
○:シボの模様がはっきり見える。×:シボの模様が確認されない。
[判定基準]
○:ホッパー内にて樹脂成分の付着が発生せず、ベント口からの多量のガス噴出もせず、かつ生産中のストランドの切れが発生していない
×:ホッパー内にて樹脂成分の付着発生、ベント口からの多量のガス噴出、または生産中のストランドの切れ発生のいずれかが起こる
[判定基準]
○:(最大のΔE)-(最小のΔE)が0.5未満
△:(最大のΔE)-(最小のΔE)が0.5以上1.0未満
×:(最大のΔE)-(最小のΔE)が1.0以上
(A)結晶性ポリアミド樹脂:ナイロン6、M2000、MEIDA社製、相対粘度2.0
(B)半芳香族非晶性ポリアミド樹脂:ヘキサメチレンテレフタルアミド/ヘキサメチレンイソフタルアミド(6T/6I樹脂)、G21、EMS社製、相対粘度2.1
(C-1)ガラス繊維:ECS03T-275H、日本電気硝子社製、繊維径10μm、カット長3.0mm
(C-2)針状ワラストナイト:NYGLOS-8 NYCO社製、平均繊維径8μm、平均繊維長136μm
(C-3)板状晶の無機強化材:マイカ、S-325、レプコ社製、平均粒子径18μm、平均アスペクト比20
(D)カーボンブラックのマスターバッチ:ABF-T-9801、レジノカラー社製、ベース樹脂はAS樹脂、カーボンブラックを45質量%含有
(E)銅化合物:臭化第二銅
銅化合物を水溶液にして投入した場合、表1に添加方法A、銅化合物をそのまま直接投入した場合、表1に添加方法Bと記した。添加方法Aでは、銅化合物は臭化第二銅を水溶液にして用いた。銅化合物の水溶液の濃度は、表1記載の濃度に調製した。
表1に示す組成になるように、無機強化材以外の各原料を予め混合して二軸押出機のホッパー部から投入し、各強化材は二軸押出機のサイドフィーダーから投入した。二軸押出機のシリンダー温度280℃、スクリュー回転数180rpmにてコンパウンドを実施し、ペレットを作成した。得られたペレットは、熱風乾燥機にて水分率0.05%以下になるまで乾燥後、種々の特性を評価した。評価結果を表1に示す。
Claims (1)
- (A)ポリカプラミド樹脂を主成分とする結晶性ポリアミド樹脂、(B)半芳香族非晶性ポリアミド樹脂、(C)無機強化材、(D)カーボンブラックのマスターバッチ、及び(E)銅化合物を含有するポリアミド樹脂組成物の製造方法であって、
該ポリアミド樹脂組成物は、
(C)無機強化材として、(C-1)ガラス繊維、(C-2)針状ワラストナイト、及び(C-3)板状晶の無機強化材を含み、
ポリアミド樹脂組成物の水分率0.05%以下でのメルトマスフローレイト(MFR)が4.0g/10分以上、13.0g/10分未満であり(なお、メルトマスフローレイト(MFR)は、JIS K 7210-1:2014に準じて275℃、2160g荷重で測定した値である。)、
ポリアミド樹脂組成物の示差走査熱量計(DSC)で測定した降温結晶化温度(TC2)が、180℃以上、185℃以下であり、
(A)と(B)との質量比が0.5<(B)/(A)≦0.8を満足し、
(A)、(B)、(C)、及び(D)の合計を100質量部としたとき、(E)の含有量が、0.001~0.1質量部であり、各成分の含有量が下記式を満足し、
30質量部≦(A)+(B)+(D)≦60質量部
13質量部≦(B)≦23質量部
1質量部≦(D)≦5質量部
20質量部≦(C-1)≦40質量部
8質量部≦(C-2)≦25質量部
8質量部≦(C-3)≦25質量部
40質量部≦(C-1)+(C-2)+(C-3)≦70質量部
(E)銅化合物は、濃度を0.04質量%~1.0質量%とした銅化合物の水溶液とし、(A)ポリカプラミド樹脂を主成分とする結晶性ポリアミド樹脂、(B)半芳香族非晶性ポリアミド樹脂、(D)カーボンブラックのマスターバッチ、及び(E)銅化合物の分散液を予め混合して押出機のホッパー部に投入し、(C)無機強化材を押出機にサイドフィード方式によって投入することを特徴とするポリアミド樹脂組成物の製造方法。
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