JP5165466B2 - 半芳香族ポリアミド成形組成物及びその使用 - Google Patents
半芳香族ポリアミド成形組成物及びその使用 Download PDFInfo
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- JP5165466B2 JP5165466B2 JP2008145140A JP2008145140A JP5165466B2 JP 5165466 B2 JP5165466 B2 JP 5165466B2 JP 2008145140 A JP2008145140 A JP 2008145140A JP 2008145140 A JP2008145140 A JP 2008145140A JP 5165466 B2 JP5165466 B2 JP 5165466B2
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- polyamide molding
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- 239000000203 mixture Substances 0.000 title claims description 115
- 238000000465 moulding Methods 0.000 title claims description 72
- 229920006012 semi-aromatic polyamide Polymers 0.000 title description 6
- 239000004952 Polyamide Substances 0.000 claims description 74
- 229920002647 polyamide Polymers 0.000 claims description 74
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 62
- 238000000034 method Methods 0.000 claims description 55
- 150000004985 diamines Chemical class 0.000 claims description 54
- 229920001577 copolymer Polymers 0.000 claims description 40
- -1 aliphatic diamines Chemical class 0.000 claims description 39
- 239000000178 monomer Substances 0.000 claims description 39
- 239000000835 fiber Substances 0.000 claims description 38
- 239000003365 glass fiber Substances 0.000 claims description 37
- 230000008569 process Effects 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 27
- 230000008018 melting Effects 0.000 claims description 24
- 238000002844 melting Methods 0.000 claims description 24
- 238000010521 absorption reaction Methods 0.000 claims description 23
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 22
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- 229920001400 block copolymer Polymers 0.000 claims description 18
- 125000004432 carbon atom Chemical group C* 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 16
- 229920000642 polymer Polymers 0.000 claims description 16
- 239000003063 flame retardant Substances 0.000 claims description 15
- 229920001955 polyphenylene ether Polymers 0.000 claims description 15
- 239000004609 Impact Modifier Substances 0.000 claims description 14
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 14
- 239000000945 filler Substances 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 12
- 125000001931 aliphatic group Chemical group 0.000 claims description 11
- 150000001991 dicarboxylic acids Chemical class 0.000 claims description 11
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 10
- 125000003118 aryl group Chemical group 0.000 claims description 10
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 10
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 10
- GAGWMWLBYJPFDD-UHFFFAOYSA-N 2-methyloctane-1,8-diamine Chemical compound NCC(C)CCCCCCN GAGWMWLBYJPFDD-UHFFFAOYSA-N 0.000 claims description 9
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical compound NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 claims description 9
- 238000006068 polycondensation reaction Methods 0.000 claims description 9
- BTZVDPWKGXMQFW-UHFFFAOYSA-N Pentadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCC(O)=O BTZVDPWKGXMQFW-UHFFFAOYSA-N 0.000 claims description 8
- 150000008064 anhydrides Chemical class 0.000 claims description 8
- 150000002148 esters Chemical class 0.000 claims description 8
- QQHJDPROMQRDLA-UHFFFAOYSA-N hexadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCC(O)=O QQHJDPROMQRDLA-UHFFFAOYSA-N 0.000 claims description 8
- BNJOQKFENDDGSC-UHFFFAOYSA-N octadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCC(O)=O BNJOQKFENDDGSC-UHFFFAOYSA-N 0.000 claims description 8
- HQHCYKULIHKCEB-UHFFFAOYSA-N tetradecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCC(O)=O HQHCYKULIHKCEB-UHFFFAOYSA-N 0.000 claims description 8
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 7
- 239000004917 carbon fiber Substances 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- QFTYSVGGYOXFRQ-UHFFFAOYSA-N dodecane-1,12-diamine Chemical compound NCCCCCCCCCCCCN QFTYSVGGYOXFRQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 6
- 150000001413 amino acids Chemical class 0.000 claims description 6
- 150000003951 lactams Chemical class 0.000 claims description 6
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 6
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 6
- 239000001361 adipic acid Substances 0.000 claims description 5
- 235000011037 adipic acid Nutrition 0.000 claims description 5
- 239000011324 bead Substances 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 5
- 239000012779 reinforcing material Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- MRERMGPPCLQIPD-NBVRZTHBSA-N (3beta,5alpha,9alpha,22E,24R)-3,5,9-Trihydroxy-23-methylergosta-7,22-dien-6-one Chemical compound C1C(O)CCC2(C)C(CCC3(C(C(C)/C=C(\C)C(C)C(C)C)CCC33)C)(O)C3=CC(=O)C21O MRERMGPPCLQIPD-NBVRZTHBSA-N 0.000 claims description 4
- PXGZQGDTEZPERC-UHFFFAOYSA-N 1,4-cyclohexanedicarboxylic acid Chemical compound OC(=O)C1CCC(C(O)=O)CC1 PXGZQGDTEZPERC-UHFFFAOYSA-N 0.000 claims description 4
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 claims description 4
- OBETXYAYXDNJHR-UHFFFAOYSA-N 2-Ethylhexanoic acid Chemical compound CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 4
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 4
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000539 dimer Substances 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000975 dye Substances 0.000 claims description 4
- ATJCASULPHYKHT-UHFFFAOYSA-N hexadecane-1,16-diamine Chemical compound NCCCCCCCCCCCCCCCCN ATJCASULPHYKHT-UHFFFAOYSA-N 0.000 claims description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 4
- CJYCVQJRVSAFKB-UHFFFAOYSA-N octadecane-1,18-diamine Chemical compound NCCCCCCCCCCCCCCCCCCN CJYCVQJRVSAFKB-UHFFFAOYSA-N 0.000 claims description 4
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 claims description 4
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical group NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 4
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 4
- MSVPBWBOFXVAJF-UHFFFAOYSA-N tetradecane-1,14-diamine Chemical compound NCCCCCCCCCCCCCCN MSVPBWBOFXVAJF-UHFFFAOYSA-N 0.000 claims description 4
- LWBHHRRTOZQPDM-UHFFFAOYSA-N undecanedioic acid Chemical compound OC(=O)CCCCCCCCCC(O)=O LWBHHRRTOZQPDM-UHFFFAOYSA-N 0.000 claims description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 4
- JCUZDQXWVYNXHD-UHFFFAOYSA-N 2,2,4-trimethylhexane-1,6-diamine Chemical compound NCCC(C)CC(C)(C)CN JCUZDQXWVYNXHD-UHFFFAOYSA-N 0.000 claims description 3
- IGSBHTZEJMPDSZ-UHFFFAOYSA-N 4-[(4-amino-3-methylcyclohexyl)methyl]-2-methylcyclohexan-1-amine Chemical compound C1CC(N)C(C)CC1CC1CC(C)C(N)CC1 IGSBHTZEJMPDSZ-UHFFFAOYSA-N 0.000 claims description 3
- DZIHTWJGPDVSGE-UHFFFAOYSA-N 4-[(4-aminocyclohexyl)methyl]cyclohexan-1-amine Chemical compound C1CC(N)CCC1CC1CCC(N)CC1 DZIHTWJGPDVSGE-UHFFFAOYSA-N 0.000 claims description 3
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 3
- BHHGXPLMPWCGHP-UHFFFAOYSA-N Phenethylamine Chemical compound NCCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-N 0.000 claims description 3
- QLZHNIAADXEJJP-UHFFFAOYSA-N Phenylphosphonic acid Chemical compound OP(O)(=O)C1=CC=CC=C1 QLZHNIAADXEJJP-UHFFFAOYSA-N 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- QLBRROYTTDFLDX-UHFFFAOYSA-N [3-(aminomethyl)cyclohexyl]methanamine Chemical compound NCC1CCCC(CN)C1 QLBRROYTTDFLDX-UHFFFAOYSA-N 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 229920000554 ionomer Polymers 0.000 claims description 3
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical compound NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 claims description 3
- MLCHBQKMVKNBOV-UHFFFAOYSA-N phenylphosphinic acid Chemical compound OP(=O)C1=CC=CC=C1 MLCHBQKMVKNBOV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 150000003018 phosphorus compounds Chemical class 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 claims description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 2
- DPQHRXRAZHNGRU-UHFFFAOYSA-N 2,4,4-trimethylhexane-1,6-diamine Chemical compound NCC(C)CC(C)(C)CCN DPQHRXRAZHNGRU-UHFFFAOYSA-N 0.000 claims description 2
- NDXNCTAJOQSKIO-UHFFFAOYSA-N 2-butyl-2-ethylpentane-1,5-diamine Chemical compound CCCCC(CC)(CN)CCCN NDXNCTAJOQSKIO-UHFFFAOYSA-N 0.000 claims description 2
- LTHNHFOGQMKPOV-UHFFFAOYSA-N 2-ethylhexan-1-amine Chemical compound CCCCC(CC)CN LTHNHFOGQMKPOV-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- MBRGOFWKNLPACT-UHFFFAOYSA-N 5-methylnonane-1,9-diamine Chemical compound NCCCCC(C)CCCCN MBRGOFWKNLPACT-UHFFFAOYSA-N 0.000 claims description 2
- SLXKOJJOQWFEFD-UHFFFAOYSA-N 6-aminohexanoic acid Chemical compound NCCCCCC(O)=O SLXKOJJOQWFEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000005711 Benzoic acid Substances 0.000 claims description 2
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- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 claims description 2
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- XTUVJUMINZSXGF-UHFFFAOYSA-N N-methylcyclohexylamine Chemical compound CNC1CCCCC1 XTUVJUMINZSXGF-UHFFFAOYSA-N 0.000 claims description 2
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- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
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- 239000002482 conductive additive Substances 0.000 claims description 2
- YMHQVDAATAEZLO-UHFFFAOYSA-N cyclohexane-1,1-diamine Chemical compound NC1(N)CCCCC1 YMHQVDAATAEZLO-UHFFFAOYSA-N 0.000 claims description 2
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- ITZPOSYADVYECJ-UHFFFAOYSA-N n'-cyclohexylpropane-1,3-diamine Chemical compound NCCCNC1CCCCC1 ITZPOSYADVYECJ-UHFFFAOYSA-N 0.000 claims description 2
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
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Images
Classifications
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
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Description
本発明はテレフタル酸コポリアミドを基礎としたポリアミド成形組成物及びその製造方法及びその使用方法に関する。
PA6及びPA66のような公知の標準的ポリアミド類は加工しやすく、特にガラス繊維強化材又は鉱物充填材を含む場合に高い融点及び高い熱変形温度を有する。しかしながら、典型的には、それらは浸水した場合10%までの高い水分吸収を有する。濡れ又は湿性条件下を含む寸法安定性の為の厳しい要件を有する多くの適用の為にはこれらの脂肪族ポリアミドは使用することができない。水分吸収は寸法だけでなく機械的特性も変化させる。水分吸収は剛性値(stiffness values)及び強度値(strength values)をそれらの前のレベルの一部分にまで減少させる。
本発明は従って、濡れ又は湿性条件下を含む機械的特性に関してのみならず、加工可能性に関しても、とりわけ先行技術を超えた改良ポリアミド成形組成物を提供する目的に基づく。さらなる目的はこの成形組成物を主成分とする成形物及びこの成形組成物の調製方法を提供することである。
(A)30〜100質量%の少なくとも一つの10T/6Tコポリアミドであって、
(A1)1,10-デカンジアミンモノマー及びテレフタル酸から形成される40〜95mol%の10Tユニット、
(A2)1,6-ヘキサンジアミンモノマー及びテレフタル酸から形成される5〜60mol%の6Tユニット、
で構成される前記コポリアミド。
(B)0〜70質量%の強化材料及び/又は充填材。
(C)0〜50質量%の添加剤及び/又はさらなるポリマー。
ここで、成分A〜Cの全体は100%である。
-高い熱変形温度(50%のガラス繊維で強化したPAの270℃を超える融点又は260℃を超えるHDT)、
-良好な加工性(320℃未満の融点;結晶化挙動)、
-低い水分吸収(<5%、95℃で240時間浸水後)、
-水分吸収後の変わらない機械的特性(例えば、湿性弾力引張り係数>100%の乾性弾力引張り係数、湿性耐力強度又は湿性破壊応力>85%乾性耐力強度又は乾性破壊応力)
-ガラス繊維-強化生成物の良好な表面特性、
-高い寸法安定性。
式中、
R1及びR2は同一又は異なり、好ましくはC1-C8-アルキルであり、直鎖又は分岐であり、及び/又はアリールであり、
R3はC1-C10-アルキレンであり、直鎖又は分岐であり、又はC6-C10-アリーレン又はアルキルアリーレン又はアリールアルキレンであり、
Mは元素の周期表の2族又は3族の典型又は遷移金属イオンであり、
mは2又は3であり、
nは1又は3であり、
xは1又は2である。
使用される金属イオンMは好ましくはAl、Ca及びZnを含む。
TAFMER MH5010:g-MA(0.6%)エチレン-ブチレンコポリマー;三井社製
TAFMER MH7010:g-MA(0.7%)エチレン-ブチレンコポリマー;三井社製
TAFMER MH7020:g-MA(0.7%)EPコポリマー;三井製
EXXELOR VA1801:g-MA(0.7%)EPコポリマー;エクソンモービルケミカルズ社製、米国
EXXELOR VA1803:g-MA(0.5-0.9%)EPコポリマー、無定形,エクソン社製
EXXELOR VA1810:g-MA(0.5%)EPコポリマー、エクソン社製
EXXELOR MDEX 94 1 l:g-MA(0.7%)EPDM、エクソン社製
FUSABOND MN493D:g-MA(0.5%)エチレン-オクテンコポリマー、デュポン社製、米国
FUSABOND A EB560D:(g-MA)エチレン-n-ブチルアクリレートコポリマー、デュポン社製
ELVALOY、デュポン社製
生成物の製造/調製方法:
半芳香族PA10T/6Tコポリアミド(A)はそれ自体が公知の方法で調製される。適切な方法は様々な刊行物に記載されており、いくつかの可能性のある方法は以下で引用する特許文献中で議論されており、以下に議論した文献の開示はこの文献の開示への参照により本発明の成分(A)のコポリアミドの調製のための方法に関し明白に組み込まれる。:
a)5〜50質量%の濃度の成分を有する水溶液中でのジアミンとジカルボキシ酸を含む塩の形成のための塩形成段階、及び適切な場合は、20℃〜220℃の温度で、23barまでの圧力下で部分的に前反応を行い、低分子量オリゴアミドを得る。
弾力の引張り係数:
ISO 527を、速度50mm/min張力試験(非強化変形例)又は速度5mm/min(強化変形例)張力試験に使用。
ISO張力試料、標準:ISO/CD3167、A1型、170×20/10×4mm、温度23℃
横径剛性は、方向依存的な剛性及び強度の測定が可能な、BIAX試験試料(BIAX, Noss’Ovra Staff Magazine, December 2006, No. 12, volume 29, EMS-CHEMIE AG)で測定した。
ISO 527を、速度50mm/min張力試験(非強化変形例)又は速度5mm/min(強化変形例)張力試験に使用
ISO張力試料、標準:ISO/CD 3167、A1型、170×20/10×4mm、温度23℃
横径強度(横径の最終引張り強度)は方向依存的な剛性及び強度の測定が可能な、BIAX試験試料(BIAX、Noss’Ovra Staff Magazine、December 2006、No. 12、volume 29、EMS-CHEMIE AG)で測定した。
融点、融解エンタルピー及びガラス転移温度(Tg):
ISO標準11357 11 2
顆粒状材料
示差走査熱分析(DSC)は20℃/minの加熱速度を用いて行った。開始温度をガラス転移温度(Tg)という。
DIN EN ISO 307、濃度0.5質量%のm-クレゾール溶液、20℃、顆粒化材料。
ISO 75
ISO衝撃試料80×10×4
低温衝撃、破壊応力、破壊時の伸長:
VW TL 52435
低温衝撃試験は40℃、500gで行い、長軸方向の引張り試験は23℃、50%湿度、100mm/min、8×1mmチューブで行った。
DIN 73378
8×1mmチューブ
ジアミン(s)、テレフタル酸、触媒、制御剤及び水を20lのオートクレーブに入れ生成物温度まで加熱時間加熱し、圧フェーズ時間、規定の圧力を維持する。そして次にノズルを通じて放出される。予備縮合物は24時間120℃で30ミリバールの真空の下で乾燥させる。
実施例PreCから得られた予備縮合物はWerner and Pfleiderer社製の二軸押出機内で直径25mmのスクリューを用い、規定のプロセスパラメーター(バレル温度、スクリュー回転速度、処理量)で縮合される。溶解物はゾーン10において窒素流により脱揮発する。
製品は、ひも状の形態で直径3mmのダイから押し出され、ペレット化される。ペレットは24時間30ミリバールの真空下、120℃で乾燥する。
発明実施例PostC由来及び比較実施例PostC由来の縮合物又はそれぞれ、縮合材料(IE11 IE15及びCE9 CE12)はArburg Allrounder社製320 210 750射出成形機で射出成形され、規定されたゾーン1〜4のシリンダー温度及び規定された成形温度でISO張力試料をもたらす。
表4:比較実施例 CE5-CE8、PreC、PostC及びIMTSの開始重量、プロセス条件及び特性
ジアミン(s)、テレフタル酸、触媒,制御剤及び水を溶解槽の中に入れ180℃まで加熱し、モノマー混合物を均一化した後、供給容器内に放出する。塩溶液を2つの熱交換器内で継続的に258℃まで加熱し、環状反応機内で34barの圧力で維持し、続いてノズルを用いて放出する。予備縮合物を24時間、120℃で30mbarの真空下乾燥させる。
予備縮合物は発明実施例1 7におけるように表に列挙された条件下縮合される。
表5:発明実施例IE8-IE10、PreC及びPostCの開始重量、プロセス条件及び特性
発明実施例IE8-IE10から得られた縮合物、PostCはWerner and Pfleiderer社製の2軸押出機で直径25mmのスクリューを用い、規定のプロセスパラメーター(バレル温度、スクリュー回転速度、処理量)で配合した。生成物はひも状の形態で直径3mmのダイから押し出され、ペレット化される。ペレットを24時間120℃で乾燥させる。
表7:実施例IE12 IE13及び比較実施例CE10及びCE11のハイブリッド-強化複合材料の組成及び特性
表9:フラットガラス繊維で強化した複合材料の組成及び特性
(*)機械的特性は、長軸方向及び横径方向についてBIAX張力試料の助けがある射出成形の方向に関して測定した。
断面軸の比=4,
アミノシランサイズ、NITTO BOSEKI社製、日本(上記目的の為のフラットガラス繊維)
Exolit(登録商標) GP1230:有機リン塩(Clariant Produkte有限会社製)、難燃剤。
Claims (34)
- 以下の組成を有するポリアミド成形組成物:
(A)30〜100質量%の少なくともひとつのコポリアミド10T/6Tであって、
(A1)1,10-デカンジアミン及びテレフタル酸モノマーから形成される40〜95mol%の10Tユニット、
(A2)1,6-ヘキサンジアミン及びテレフタル酸モノマーから形成される5〜60mol%の6Tユニット、
で構成される、前記ポリアミド、
(B)0〜70質量%の強化材料及び/又は充填材、
(C)0〜50質量%添加剤及び/又は更なるポリマー、
成分(A)〜(C)の全体が100%であり、
ただし成分(A)において、互いに独立して、(A1)及び/又は(A2)においてはジカルボン酸の全体に対する30mol%までのテレフタル酸は、6〜36個の炭素原子を有する他の芳香族、脂肪族又は環状脂肪族ジカルボン酸によって置換することができ、
及び、ただし成分(A)において、互いに独立して、(A1)及び/又は(A2)においてはジアミンの全体に対して30mol%までの1,10-デカンジアミン及びそれぞれ1,6-ヘキサンジアミンを4〜36個の炭素原子を有する他のジアミンで置換することができ、
及び、ただし成分(A)においてモノマーの全体に対して30mol%を超えない範囲をラクタム又はアミノ酸で構成することができ、
ただし、テレフタル酸、1,6-ヘキサンジアミン及び1,10-デカンジアミンを置換するモノマーの全体の濃度が、成分(A)で使用されるモノマーの全体に対して30mol%を超えない。 - 融点及び成分(A)及び/又はポリアミド成形組成物全体のISO-R 75方法A(DIN 53 461)による変形温度がそれぞれ、260℃より高い請求項1記載のポリアミド成形組成物。
- 95℃、240時間浸水後の成分(A)及び/又はポリアミド成形組成物の全体の水分吸収が5質量%未満である、請求項1又は請求項2に記載のポリアミド成形組成物
- 弾力の引張り係数の湿性:乾性の比が0.95以上である請求項1〜3のいずれか1項記載のポリアミド成形組成物。
- 最大引張り強度の湿性:乾性の比が0.85以上である、請求項1〜4のいずれか1項記載のポリアミド成形組成物。
- 成分(A)中、(A1)画分は40〜90mol%及び(A2)画分は10〜60mol%を構成する、請求項1〜5のいずれか1項記載のポリアミド成形組成物。
- 成分(A)の10T/6Tコポリアミドのジカルボン酸がテレフタル酸からなる、請求項1〜6のいずれか1項記載のポリアミド成形組成物。
- テレフタル酸を置換する、6〜36個の炭素原子を有する他の芳香族、脂肪族又は環状脂肪族ジカルボン酸が、ナフタレンジカルボン酸(NDA)、イソフタル酸(IPS)、アジピン酸、スベリン酸、アゼライン酸、セバシン酸、ウンデカン二酸、ドデカン二酸、ブラッシル酸、テトラデカン二酸、ペンタデカン二酸、ヘキサデカン二酸、オクタデカン二酸、酸二量体、シス及び/又はトランス-シクロヘキサン-1,4-ジカルボン酸、シス及び/又はトランス-シクロヘキサン-1,3-ジカルボン酸(CHDA)、及びそれらの組み合わせからなる群から選択される、請求項1〜6のいずれか1項記載のポリアミド成形組成物。
- テレフタル酸を置換する、6〜36個の炭素原子を有する他の芳香族、脂肪族または環状脂肪族ジカルボン酸が、ナフタレンジカルボン酸(NDA)、イソフタル酸(IPS)、トランス-シクロヘキサン-1,3-ジカルボン酸(CHDA)及びそれらの組み合わせからなる群より選択され、又はドデカン二酸、ブラッシル酸、テトラデカン二酸、ペンタデカン二酸、ヘキサデカン二酸、オクタデカン二酸、酸二量体及びそれらの組み合わせからなる群から選択される、請求項8記載のポリアミド成形組成物。
- 成分(A)の10T/6Tコポリアミドのジアミンが、(A1)については1,10-デカンジアミン及び(A2)については1,6-ヘキサンジアミンからなる、請求項1〜9のいずれか1項記載のポリアミド成形組成物。
- 成分(A)における4〜36個の炭素原子を有する他のジアミンが、互いに独立して、(A1)及び/又は(A2)においてジアミンの全体に対し30mol%までの1,10-デカンジアミン及び1,6-ヘキサンジアミンをそれぞれ置換し、直鎖又は分岐脂肪族ジアミン、環状脂肪族ジアミン、アリール脂肪族ジアミン及びそれらの組み合わせからなる群より選択される、請求項1〜9のいずれか1項記載のポリアミド成形組成物。
- 直鎖又は分岐脂肪族ジアミンが、1,4-ブタンジアミン、1,5-ペンタンジアミン、2-メチル-1,5-ペンタンジアミン(MPMD)、1,8-オクタン-ジアミン(OMDA)、1,9-ノナンジアミン(NMDA)、2-メチル-1,8-オクタンジアミン(MODA)、2,2,4-トリメチル-ヘキサメチレンジアミン(TMHMD)、2,4,4-トリメチルヘキサ-メチレンジアミン(TMHMD)、5-メチル-1,9-ノナン-ジアミン、1,11-トリデカンジアミン、2-ブチル-2-エチル-1,5-ペンタンジアミン、1,12-ドデカンジアミン、1,13-トリデカンジアミン、1,14-テトラデカンジアミン、1,16-ヘキサデカンジアミン及び1,18-オクタデカンジアミンからなる群から選択される、請求項11記載のポリアミド成形組成物。
- 環状脂肪族ジアミンが、シクロヘキサンジアミン、1,3-ビス(アミノメチル)シクロヘキサン(BAC)、イソフォロンジアミン、ノルボルナンジメチレンアミン、4,4’-ジアミノ-ジシクロヘキシルメタン(PACM)、2,2-(4,4’-ジアミノ-ジシクロヘキシル)シクロプロパン(PACP)及び3,3’-ジメチル-4,4’-ジアミノジシクロヘキシルメタン(MACM)からなる群から選択される、請求項11記載のポリアミド成形組成物。
- 成分(A)における、4〜36個の炭素原子を有する他のジアミンが、互いに独立して、(A1)及び/又は(A2)においてジアミンの全体に対し30mol%までの1,10-デカンジアミン及びそれぞれ1,6-ヘキサンジアミンを置換し、2-メチル-1,5-ペンタンジアミン(MPMD)、2-メチル-1,8-オクタンジアミン(MODA)、2,2,4-トリメチルヘキサメチレンジアミン(TMHMD)、1,3-ビス(アミノメチル)シクロヘキサン(BAC)、4,4’-ジアミノ-ジシクロヘキシルメタン(PACM)、3,3’-ジメチル-4,4’-ジアミノジシクロヘキシルメタン(MACM)、及びそれらの組み合わせからなる群から選択され、又は1,12-ドデカンジアミン、1,13-トリデカンジアミン、1,14-テトラデカンジアミン、1,16-ヘキサデカンジアミン、1,18-オクタデカンジアミン及びそれらの組み合わせからなる群より選択される、請求項11記載のポリアミド成形組成物。
- 成分(A)が成分(A1)及び(A2)からなる請求項1〜14のいずれか1項記載のポリアミド成形組成物。
- ラクタム又はアミノ酸が、カプロラクタム(CL)、α,ω-アミノカプロン酸、α,ω-アミノノナン酸、α,ω-アミノウンデカン酸(AUA)、ラウロラクタム(LL)、ω-アミノドデカン酸(ADA)及びこれらの組み合わせからなる群より選択される、請求項1〜14のいずれか1項記載のポリアミド成形組成物。
- 成分(B)がガラス繊維及び/又は炭素繊維を含む、請求項1〜16のいずれか1項記載のポリアミド成形組成物。
- 成分(B)が、短繊維及び/又は連続フィラメント繊維をガラス繊維の形態で含む、請求項17記載のポリアミド成形組成物。
- 直径が10〜14μmである短繊維及び/又は連続ガラス繊維を含む、請求項18記載のポリアミド成形組成物。
- 成分(C)が以下の群:衝撃改質剤、接着促進剤又は相溶化剤、結晶化促進剤又は結晶化抑制剤、流動助剤、潤滑剤、離型剤、色素、染料及びマーカー、可塑剤、安定剤、加工補助剤、難燃剤、帯電防止剤,層状形態のナノ粒子、伝導性添加剤、重合化工程の残分から選択される添加剤及び/又はさらなるポリマーを含む、請求項1〜19のいずれか1項記載のポリアミド成形組成物。
- テレフタル酸、1,6-ヘキサンジアミン及び1,10-デカンジアミンを置換するモノマーの全体の濃度が成分(A)で使用されるモノマーの全体に対して20mol%を超えない、請求項1〜20のいずれか1項記載のポリアミド成形組成物。
- 請求項1〜21のいずれか1項記載のポリアミド成形組成物を含むポリアミド混合物。
- 請求項1〜21のいずれか1項記載のポリアミド成形組成物並びに、コポリマー、グラフトコポリマー、ブロックコポリマー及びイオノマーからなる群から選択される形態のポリフェニレンエーテルを含む、ポリアミド混合物。
- 請求項1〜21のいずれか1項記載のポリアミド成形組成物又は請求項22若しくは請求項23に記載のポリアミド混合物で構成されるペレット化材料であって、濡れ及び/又は湿性環境下での使用をするためのペレット化材料。
- 請求項1〜21のいずれか1項記載のポリアミド成形組成物で構成される又は請求項22若しくは請求項23に記載のポリアミド混合物で構成される粉末であって、平均結晶粒度が30〜200μmである上記粉末。
- その0.5質量% m-クレゾール溶液中の、20℃における粘度が1.3〜2.0の範囲であり、ポリアミド成形組成物がカルボキシ末端基:アミノ末端基の比が1:2及びそれぞれ2:1以上であることを用いて制御された、請求項25記載の粉末。
- 10T/6Tコポリアミド粒子と共に、固体又は中空ガラスビーズの形態で、平均直径20〜80μmを有するさらなる充填材を含む請求項25又は26に記載の粉末。
- 選択的レーザー焼結法において使用する為の請求項25に記載の粉末。
- 請求項1〜21のいずれか1項記載のポリアミド成形組成物を使用し、請求項22若しくは23に記載のポリアミド混合物を使用し、請求項1〜21のいずれか1項記載のポリアミド成形組成物又は請求項22若しくは請求項23に記載のポリアミド混合物で構成されるペレット化材料を使用し、又は請求項1〜21のいずれか1項記載のポリアミド成形組成物又は請求項22若しくは請求項23に記載のポリアミド混合物で構成される粉末を使用して生産された成形物。
- 請求項1〜21のいずれか1項記載のポリアミド成形組成物の製造方法であって、成分(A)の調製中に0.005〜1.5質量%の比率で少なくとも一つのポリ縮合触媒をモノマー混合物へ加えることを含む、上記方法。
- ポリ縮合触媒が、リン酸、亜リン酸、次亜リン酸、フェニルホスホン酸及びフェニルホスフィン酸から選択されるリン化合物及び/又はそれらの1〜3価のカチオンとの塩及び/又はそれらのエステル及びそれらの混合物からなる群から選択される、請求項30に記載の方法。
- ポリ縮合触媒が、半芳香族10T/6Tコポリアミド(A)に対し100〜500ppmのリンとなる量で次亜燐酸及び次亜リン酸水素ナトリウム一水和物を含む請求項30又は31に記載の方法。
- ジアミンの損失を補填する為に全体のジアミンに対して1〜8質量%の過剰のジアミンをモノマー混合物に加える、請求項30〜32のいずれか1項記載の方法。
- 分子量、相対的粘度及びそれぞれ流動性又はMVRを制御する為に制御剤を混合物及び/又は予備縮合物に加え、前記制御剤には一酸塩基又はモノアミンが含まれ、前記一酸塩基又はモノアミンは、以下の群:酢酸、プロピオン酸、酪酸、吉草酸、カプロン酸、ラウリン酸、ステアリン酸、2-エチルカプロン酸、シクロカプロン酸、安息香酸、ブチルアミン、ペンチルアミン、ヘキシルアミン、2-エチルヘキシルアミン、n-オクチルアミン、n-ドデシルアミン、n-テトラデシルアミン、n-ヘキサデシルアミン、ステアリルアミン、シクロヘキシルアミン、3-(シクロヘキシルアミノ)プロピルアミン、メチルシクロヘキシルアミン、ジメチルシクロヘキシルアミン、ベンジルアミン、2-フェニルエチルアミン及びそれぞれそれらの組み合わせから選択される脂肪族、環状脂肪族若しくは芳香族モノカルボン酸又はモノアミン又は無水物、イソシアン酸塩、ハロゲン化アシル又はエステル及びそれぞれこれらの組み合わせから選択されるアミノ基又は酸性基と反応することができる単官能性化合物から選択され、使用した制御剤の量が10〜200mmol/kg制御剤/ポリマーである、請求項30〜33のいずれか1項記載の方法。
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US7927710B2 (en) | 2011-04-19 |
BRPI0804185B1 (pt) | 2018-12-04 |
EP1988113B1 (de) | 2009-10-14 |
KR100981404B1 (ko) | 2010-09-10 |
CA2630702C (en) | 2015-12-08 |
SG147407A1 (en) | 2008-11-28 |
MY144075A (en) | 2011-08-15 |
EP1988113A1 (de) | 2008-11-05 |
CN106987119A (zh) | 2017-07-28 |
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