CN114585688A - 半芳香族聚酰胺树脂组合物、及金属镀敷成形体 - Google Patents
半芳香族聚酰胺树脂组合物、及金属镀敷成形体 Download PDFInfo
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- CN114585688A CN114585688A CN202080071623.1A CN202080071623A CN114585688A CN 114585688 A CN114585688 A CN 114585688A CN 202080071623 A CN202080071623 A CN 202080071623A CN 114585688 A CN114585688 A CN 114585688A
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- Prior art keywords
- semi
- polyamide resin
- aromatic polyamide
- acid
- resin composition
- Prior art date
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- 229920006012 semi-aromatic polyamide Polymers 0.000 title claims abstract description 143
- 238000007747 plating Methods 0.000 title claims abstract description 86
- 239000011342 resin composition Substances 0.000 title claims abstract description 77
- 229910052751 metal Inorganic materials 0.000 title claims description 78
- 239000002184 metal Substances 0.000 title claims description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011256 inorganic filler Substances 0.000 claims abstract description 23
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000010521 absorption reaction Methods 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 238000000113 differential scanning calorimetry Methods 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims description 88
- 239000011347 resin Substances 0.000 claims description 88
- -1 styrene-ethylene-butylene-styrene Chemical group 0.000 claims description 58
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 22
- 229920001971 elastomer Polymers 0.000 claims description 19
- 239000000806 elastomer Substances 0.000 claims description 16
- 229920000089 Cyclic olefin copolymer Polymers 0.000 claims description 15
- 150000007934 α,β-unsaturated carboxylic acids Chemical class 0.000 claims description 14
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 13
- 239000005977 Ethylene Substances 0.000 claims description 13
- 229920001577 copolymer Polymers 0.000 claims description 12
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 12
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000004711 α-olefin Substances 0.000 claims description 8
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical class [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 6
- 229920006132 styrene block copolymer Polymers 0.000 claims description 6
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical class [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 4
- 238000005476 soldering Methods 0.000 abstract description 19
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 55
- 238000000034 method Methods 0.000 description 38
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 32
- 238000012360 testing method Methods 0.000 description 25
- 229920000642 polymer Polymers 0.000 description 23
- 125000004432 carbon atom Chemical group C* 0.000 description 21
- 239000004952 Polyamide Substances 0.000 description 19
- 229920002647 polyamide Polymers 0.000 description 19
- 239000000243 solution Substances 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
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- 239000000178 monomer Substances 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 229920002554 vinyl polymer Polymers 0.000 description 12
- 150000001993 dienes Chemical class 0.000 description 11
- 238000000465 moulding Methods 0.000 description 11
- 238000002156 mixing Methods 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 9
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- 239000002994 raw material Substances 0.000 description 9
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- 238000005530 etching Methods 0.000 description 8
- 125000003277 amino group Chemical group 0.000 description 7
- 239000003963 antioxidant agent Substances 0.000 description 7
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 7
- 239000007822 coupling agent Substances 0.000 description 7
- 238000001746 injection moulding Methods 0.000 description 7
- 239000003607 modifier Substances 0.000 description 7
- 229910052759 nickel Inorganic materials 0.000 description 7
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- 230000000052 comparative effect Effects 0.000 description 6
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- 150000003951 lactams Chemical class 0.000 description 6
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical compound NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229920005992 thermoplastic resin Polymers 0.000 description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N 1-nonene Chemical compound CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 5
- HASUJDLTAYUWCO-UHFFFAOYSA-N 2-aminoundecanoic acid Chemical compound CCCCCCCCCC(N)C(O)=O HASUJDLTAYUWCO-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 5
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- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 5
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 238000007740 vapor deposition Methods 0.000 description 5
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N 1-Heptene Chemical compound CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 4
- AFFLGGQVNFXPEV-UHFFFAOYSA-N 1-decene Chemical compound CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 description 4
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- ADOBXTDBFNCOBN-UHFFFAOYSA-N 1-heptadecene Chemical compound CCCCCCCCCCCCCCCC=C ADOBXTDBFNCOBN-UHFFFAOYSA-N 0.000 description 4
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 description 4
- HFDVRLIODXPAHB-UHFFFAOYSA-N 1-tetradecene Chemical compound CCCCCCCCCCCCC=C HFDVRLIODXPAHB-UHFFFAOYSA-N 0.000 description 4
- GAGWMWLBYJPFDD-UHFFFAOYSA-N 2-methyloctane-1,8-diamine Chemical compound NCC(C)CCCCCCN GAGWMWLBYJPFDD-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 4
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- 239000000654 additive Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 4
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- 239000000835 fiber Substances 0.000 description 4
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- NHLUYCJZUXOUBX-UHFFFAOYSA-N nonadec-1-ene Chemical compound CCCCCCCCCCCCCCCCCC=C NHLUYCJZUXOUBX-UHFFFAOYSA-N 0.000 description 4
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical compound CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 4
- GUOSQNAUYHMCRU-UHFFFAOYSA-N 11-Aminoundecanoic acid Chemical compound NCCCCCCCCCCC(O)=O GUOSQNAUYHMCRU-UHFFFAOYSA-N 0.000 description 3
- 238000005160 1H NMR spectroscopy Methods 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
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- 239000004698 Polyethylene Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
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Abstract
本发明提供一种以良好镀敷性、低吸水性、耐回流焊接性优异的半芳香族聚酰胺树脂组合物。本发明的半芳香族聚酰胺树脂组合物,相对于半芳香族聚酰胺(A)100质量份,含有无机填充材料(B)10~200质量份和韧性改良材料(C)2~30质量份,该半芳香族聚酰胺树脂(A)满足下述(a)、(b),(a)通过差示扫描量热法(DSC)测得的熔点(Tm)为280℃以上,(b)80℃、95%RH平衡吸水率为3.5%以下。
Description
技术领域
本发明涉及一种良好镀敷性、低吸水性和耐回流焊接性优异的半芳香族聚酰胺树脂组合物。
背景技術
聚酰胺树脂运用其优良的特性和熔融成形的容易性而一直被用于衣料用、产业材料用纤维、工程塑料等。近年来,随着在各领域的技术发展,聚酰胺树脂的用途进一步扩大,在从发动机周边的汽车部件到以智能手机为代表的电气电子部件的各种用途中得到使用。
随着各种技术的发展,在电气电子机器、办公自动化机器中高性能化不断发展,汽车领域中也需要抑制将电机用于驱动源等由各种部件产生的电磁波对周边部件或人体产生的影响。
为了应对这些问题,已经进行了对各种机器的构成部件赋予电磁波屏蔽性的研究,已经使用了电磁波屏蔽性优异的金属、混合有导电性填料的树脂。虽然用这些方法也可以实现电磁波屏蔽,但在汽车的油耗改善、产品轻量化、树脂加工性这样的方面存在问题。
另一方面,作为对机器的构成部件赋予电磁波屏蔽性的方法,已知有在树脂成形品的表面实施金属蒸镀或金属镀敷的方法。与以金属构成部件本身相比,更容易轻量化,并能提供充分的电磁波屏蔽性,因此被用于各种领域中。
对于树脂的金属蒸镀和金属镀敷技术已经进行了各种开发。专利文献1公开了一种由聚酰胺与无机填充剂、改性苯乙烯·烯烃系共聚物构成的与金属镀层之间的密贴性优异的聚酰胺树脂组合物。然而,由于该文献中记载的聚酰胺树脂组合物的熔点低于280℃,因此难以承受在基盘部件的制造中使用的回流焊接工序。
专利文献2公开了含有聚酰胺树脂、苯乙烯系树脂和填料的金属蒸镀用树脂组合物。但是,该文献中记载的金属蒸镀用树脂组合物是记载了与通过金属蒸镀技术形成的金属膜具有良好的密贴性的物质,金属膜的形成工艺与本发明的金属镀敷技术有本质上的不同。另外,实施例中记载的金属蒸镀用树脂组合物的熔点均低于280℃,难以耐受回流焊接工序。
专利文献3公开了一种镀层形成用树脂组合物,其含有由对苯二甲酸和具有碳原子数为4~25的亚烷基的二胺成分构成的半芳香族聚酰胺及无机填料。但是,在该文献中记载的树脂组合物中,没有提及通过韧性改良材料进一步提高镀敷密贴性的效果。
专利文献4公开了一种成形体,该成形体的表面具有金属层,该成形体由聚酰胺树脂组合物得到,该聚酰胺树脂组合物由对苯二甲酸、1,9-壬二胺构成的聚酰胺树脂及填充剂构成。然而,该文献中记载述的树脂组合物限定了聚酰胺树脂。
专利文献5公开了使用在选自聚酰胺10T、聚酰胺9T、聚酰胺6T、聚酰胺4T、或聚邻苯二甲酰胺中的任一种的半芳香族聚酰胺树脂中混合了填充剂的树脂组合物的无电解镀敷层的形成方法。但是,该文献记载的技术在使用树脂组合物对实施镀敷的基体进行成形时,需要将模具温度设定为180~240℃,在设备方面存在限制。
如上所述,关于对树脂进行的金属蒸镀、金属镀敷,已经做出了各种发明,但是存在各种问题和限制。
现有技术文献
专利文献
专利文献1:日本特公平8-11782号公报
专利文献2:日本特开2006-131821号公报
专利文献3:日本专利第3009707号公报
专利文献4:日本专利第3400133号公报
专利文献5:日本专利第6190154号公报
发明内容
发明所要解决的问题
本发明是鉴于这样的现有技术的现状而创制出的,其目的在于提供一种良好镀敷性、低吸水性和耐回流焊接性优异的半芳香族聚酰胺树脂组合物。
用于解决问题的手段
本发明人为了达到上述目的,除了半芳香族聚酰胺树脂的组成以外,还对填充剂、韧性改良材料的种类、混合量进行了深入研究,结果实现了提供一种良好镀敷性、低吸水性、耐回流焊接性优异的半芳香族聚酰胺树脂组合物。
即,本发明具有以下构成。
(1)一种半芳香族聚酰胺树脂组合物,相对于半芳香族聚酰胺(A)100质量份,含有无机填充材料(B)10~200质量份以及韧性改良材料(C)2~30质量份,所述半芳香族聚酰胺树脂(A)满足下述(a)、(b),
(a)通过差示扫描量热法(DSC)测定的熔点(Tm)为280℃以上,
(b)80℃、95%RH平衡吸水率为3.5%以下。
(2)根据(1)所述的半芳香族聚酰胺树脂组合物,韧性提高材料(C)为选自烯烃系共聚物及苯乙烯系弹性体中的至少一种。
(3)根据(2)所述的半芳香族聚酰胺树脂组合物,烯烃系共聚物是选自(乙烯和/或丙烯)·α-烯烃系共聚物、(乙烯和/或丙烯)·(α,β-不饱和羧酸和/或不饱和羧酸酯)系共聚物中的至少一种。
(4)根据(2)或(3)所述的半芳香族聚酰胺树脂组合物,苯乙烯系弹性体为苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物。
(5)根据(1)~(4)中任一项所述的半芳香族聚酰胺树脂组合物,无机填充材料(B)含有硅酸铝盐、硅酸钙盐。
(6)一种金属镀敷成形体,使用了(1)~(5)中任一项所述的半芳香族聚酰胺树脂组合物。
发明的效果
根据本发明,可以提供一种具有良好镀敷性、低吸水性和耐回流焊接性的半芳香族聚酰胺树脂组合物,以及使用该半芳香族聚酰胺树脂组合物的镀敷成形体。
具体实施方式
以下,对本发明的半芳香族聚酰胺树脂组合物进行说明。
本发明中使用的半芳香族聚酰胺树脂(A)没有特别限定,是分子中具有酰胺键(-CONH-)、且具有芳香环(苯环)的半芳香族聚酰胺。
作为半芳香族聚酰胺的一个例子,可以举出6T系聚酰胺(例如由对苯二甲酸/间苯二甲酸/六亚甲基二胺构成的聚酰胺6T/6I、由对苯二甲酸/己二酸/六亚甲基二胺构成的聚酰胺6T/66、由对苯二甲酸/间苯二甲酸/己二酸/六亚甲基二胺构成的聚酰胺6T/6I/66、由对苯二甲酸/六亚甲基二胺/2-甲基-1,5-五亚甲基二胺构成的聚酰胺6T/M-5T、由对苯二甲酸/六亚甲基二胺/ε-己内酰胺构成的聚酰胺6T/6、由对苯二甲酸/六亚甲基二胺/四亚甲基二胺构成的聚酰胺6T/4T)、9T系聚酰胺(对苯二甲酸/1,9-壬二胺/2-甲基-1,8-辛二胺)、10T系聚酰胺(对苯二甲酸/1,10-癸二胺)、12T系聚酰胺(对苯二甲酸/1,12-十二烷二胺)、由癸二酸/对二甲苯二胺构成的聚酰胺等。
本发明中使用的半芳香族聚酰胺树脂(A)的通过差示扫描量热法(DSC)测定的熔点(Tm)需要为280℃以上。另外,熔点(Tm)优选为285℃以上,更优选为290℃以上。Tm小于上述下限时,通过回流焊接工序对使用了本发明的半芳香族聚酰胺树脂组合物的成形体进行加工时,成形体有发生熔融或变形的可能性。作为Tm的上限,优选为340℃以下,更优选为330℃以下,进一步优选为320℃以下。Tm超过上述上限时,成形加工时的加工温度变得极高,有产生由于热而导致树脂分解的可能性。通过差示扫描量热法(DSC)的测定将在下面的实施例的项目中说明。
本发明中使用的半芳香族聚酰胺树脂(A)的用下述实施例的项目中说明的方法测定的80℃、95%RH平衡吸水率需要为3.5%以下。此外,80℃、95%RH平衡吸水率优选为3.0%以下。当80℃、95%RH平衡吸水率超过上述上限时,当使用了如上所述的半芳香族聚酰胺树脂组合物的成形体通过焊料反流工序进行加工时,成形体中的表面有可能由于成形体中的水分的膨胀而发生膨胀,此外有可能由成形体的尺寸变化导致产生组装不良。
作为本发明中使用的半芳香族聚酰胺树脂(A),从80℃、95%RH平衡吸水率的观点出发,优选是以下的半芳香族聚酰胺树脂。
半芳香族聚酰胺树脂(A)优选为含有50~100摩尔%的由碳原子数为6~12的二胺和对苯二甲酸构成的重复单元、以及0~50摩尔%的由碳原子数10以上的氨基羧酸或由碳原子数10以上的内酰胺构成的重复单元的半芳香族聚酰胺树脂,更优选为含有50~98摩尔%的由碳原子数6~12的二胺和对苯二甲酸构成的重复单元、以及2~50摩尔%的由碳原子数10以上的氨基羧酸或由碳原子数10以上的内酰胺构成的重复单元的半芳香族聚酰胺树脂,进一步优选为含有55~98摩尔%的由碳原子数6~12的二胺和对苯二甲酸构成的重复单元、以及2~45摩尔%的由碳原子数10以上的氨基羧酸或由碳原子数10以上的内酰胺构成的重复单元的半芳香族聚酰胺树脂。
半芳香族聚酰胺树脂(A)中的由碳原子数6~12的二胺和对苯二甲酸构成的重复单元的比例低于50摩尔%时,存在发生由于Tm降低而导致回流焊接工序中的成形体的熔融、变形的可能性。另一方面,由于可以适度地提高半芳香族聚酰胺树脂(A)的Tm,所以更优选使半芳香族聚酰胺树脂(A)中的由碳原子数6~12的二胺和对苯二甲酸构成的重复单元的比例为55摩尔%以上,进一步优选使之为60摩尔%以上。
作为构成半芳香族聚酰胺树脂(A)的碳原子数6~12的二胺成分,可以举出1,6-六亚甲基二胺、1,7-七亚甲基二胺、1,8-八亚甲基二胺、1,9-九亚甲基二胺、2-甲基-1,8-八亚甲基二胺、1,10-十亚甲基二胺、1,11-十一亚甲基二胺、1,12-十二亚甲基二胺等。这些可以单独使用,也可以多个使用。
作为构成半芳香族聚酰胺树脂(A)的碳原子数10以上的氨基羧酸或碳原子数10以上的内酰胺,优选碳原子数11~18的氨基羧酸或内酰胺。其中,优选11-氨基十一烷酸、十一烷内酰胺、12-氨基十二烷酸、12-月桂内酰胺。从80℃、95%RH平衡吸水率的观点出发,作为共聚成分,优选将碳原子数11~18的氨基羧酸或碳原子数11~18的内酰胺中的一种或多种共聚。
本发明中使用的半芳香族聚酰胺树脂(A)中,可以以结构单元中50摩尔%以下共聚其他成分。作为可以共聚的其他二胺成分,可以举出如1,13-十三亚甲基二胺、1,16-十六亚甲基二胺、1,18-十八亚甲基二胺、2,2,4(或2,4,4)-三甲基六亚甲基二胺这样的脂肪族二胺、如哌嗪、环己烷二胺、双(3-甲基-4-氨基己基)甲烷、双-(4,4’-氨基环己基)甲烷、异佛尔酮二胺这样的脂环式二胺、间苯二甲胺、对苯二甲胺、对苯二胺、间苯二胺等芳香族二胺以及它们的氢化物等。
作为可以共聚的其他酸成分,可以举出间苯二甲酸、邻苯二甲酸、1,5-萘二甲酸、2,6-萘二甲酸、4,4’-二苯基二羧酸、2,2’-二苯基二羧酸、4,4’-二苯基醚二羧酸、间苯二甲酸-5-磺酸钠、5-羟基间苯二甲酸等芳香族二羧酸、富马酸、马来酸、琥珀酸、衣康酸、己二酸、壬二酸、癸二酸、1,11-十一烷二酸、1,12-十二烷二酸、1,14-十四烷二酸、1,18-十八烷二酸、1,4-环己烷二羧酸、1,3-环己烷二羧酸、1,2-环己烷二羧酸、4-甲基-1,2-环己烷二羧酸、二聚酸等脂肪族或脂环族二羧酸等。
此外,作为可以共聚的其他成分,可以举出ε-己内酰胺等。
本发明中使用的半芳香族聚酰胺树脂(A),优选是含有50~100摩尔%的由六亚甲基二胺和对苯二甲酸构成的重复单元、以及0~50摩尔%的由氨基十一烷酸或十一烷内酰胺构成的重复单元的半芳香族聚酰胺树脂,更优选是含有50~98摩尔%的由六亚甲基二胺和对苯二甲酸构成的重复单元、以及2~50摩尔%的由氨基十一烷酸或十一烷内酰胺构成的重复单元的半芳香族聚酰胺树脂,进一步优选是含有55~80摩尔%的由六亚甲基二胺和对苯二甲酸构成的重复单元、以及20~45摩尔%的由氨基十一烷酸或十一烷内酰胺构成的重复单元的半芳香族聚酰胺树脂,特别优选是含有60~70摩尔%的由六亚甲基二胺和对苯二甲酸构成的重复单元、30~40摩尔%的由氨基十一烷酸或十一烷内酰胺构成的重复单元的半芳香族聚酰胺树脂。
当半芳香族聚酰胺树脂(A)中的由六亚甲基二胺和对苯二甲酸构成的重复单元的比例低于50摩尔%时,存在发生由于Tm降低而导致回流焊接工序中的成形体熔融、变形的可能性。另一方面,通过使半芳香族聚酰胺树脂(A)中的由六亚甲基二胺和对苯二甲酸构成的重复单元的比例为55~80摩尔%,可以控制半芳香族聚酰胺树脂(A)的结晶性、分子运动性,可以适度提高Tm,因此优选。此外,通过使半芳香族聚酰胺树脂(A)中的由六亚甲基二胺和对苯二甲酸构成的重复单元的比例为60~70摩尔%,以及作为共聚成分使用的由氨基十一烷酸或十一烷内酰胺构成的重复单元的比例为30~40摩尔%,不仅可以将Tm控制在300℃~320℃的范围,可以容易进行成形加工,而且可以使80℃、95%RH平衡吸水率为3.5%以下,可以得到优异的耐回流焊接性,因此进一步优选。
作为在制造半芳香族聚酰胺树脂(A)时使用的催化剂,可以举出磷酸、亚磷酸、次磷酸或其金属盐或铵盐、酯。作为金属盐的金属种类,具体地可以举出钾、钠、镁、钒、钙、锌、钴、锰、锡、钨、锗、钛、锑等。作为酯,可以举出乙酯、异丙酯、丁酯、己酯、异癸酯、十八酯、癸酯、硬脂酯、苯酯等。此外,基于提高熔融滞留稳定性的观点,优选添加氢氧化钠、氢氧化钾、氢氧化镁等碱性化合物。
半芳香族聚酰胺树脂(A)的在96%浓硫酸中20℃下测定的相对粘度(RV)优选是0.4~4.0,更优选是1.0~3.0,进一步优选是1.5~2.5。作为使聚酰胺的相对粘度在一定范围的方法,可以举出调整分子量的手段。
作为半芳香族聚酰胺树脂(A)的末端羧基浓度、末端氨基浓度,分别优选为0~200eq/ton、0~100eq/ton。末端羧基浓度、末端氨基浓度超过200eq/ton时,存在在成形加工时促进凝胶化、劣化的可能性。
半芳香族聚酰胺树脂(A)可以通过调整氨基量和羧基之间的摩尔比并进行缩聚的方法或添加封端剂的方法来调整聚酰胺的末端基量以及分子量。
作为添加封端剂的时期,可以举出装入原料时、聚合引发时、聚合后期、或聚合结束时。作为封端剂,只要是与聚酰胺末端的氨基或羧基具有反应性的单官能性化合物,就没有特别的限制,但可以使用单羧酸或单胺、邻苯二甲酸酐等酸酐、单异氰酸酯、单酸卤化物、单酯类、单醇类等。作为封端剂,例如可以举出乙酸、丙酸、酪酸、戊酸、己酸、辛酸、月桂酸、十三烷酸、肉豆蔻酸、棕榈酸、硬脂酸、新戊酸、异丁酸等脂肪族单羧酸;环己基羧酸等脂环式单羧酸;苯甲酸、甲基苯甲酸、α-萘羧酸、β-萘羧酸、甲基萘羧酸、苯基乙酸等芳香族单羧酸;马来酸酐、邻苯二甲酸酐、六氢邻苯二甲酸酐等酸酐;甲胺、乙胺、丙胺、丁胺、己胺、辛胺、癸胺、硬脂胺、二甲胺、二乙胺、二丙胺、二丁胺等脂肪族单胺;环己胺、二环己胺等脂环式单胺;苯胺、甲苯胺、二苯胺、萘胺等芳香族单胺等。
半芳香族聚酰胺树脂(A)可以通过以往公知的方法制造,例如,可以通过使原料单体进行共缩聚反应而容易地合成。共缩聚反应的顺序没有特别的限定,可以使全部的原料单体一次反应,也可以先使一部分的原料单体反应,接着使剩余的原料单体反应。此外,聚合方法没有特别的限定,可以通过连续的工序进行从原料装入到聚合物制作的工序,也可以使用在一次制作低聚物后,在其他工序中通过挤出机等进行聚合,或者通过固相聚合使低聚物高分子量化等方法。通过调整原料单体的装入比率,可以控制合成的共聚聚酰胺中的各结构单元的比例。
本发明中使用的无机填充材料(B)是为了提高半芳香族聚酰胺树脂组合物的金属镀敷密贴性、强度、尺寸稳定性而混合的材料,使用选自纤维状填充材料和非纤维状填充材料中的至少1种。作为纤维状填充材料,例如可以举出玻璃纤维、碳纤维、硼纤维、陶瓷纤维、金属纤维、钛酸钾晶须、硼酸铝晶须、氧化锌晶须、碳酸钙晶须、硫酸镁晶须、纤维状硅灰石等。作为非纤维状填充材料,例如可以举出硅酸铝盐(高岭土)、硅酸钙盐(硅灰石)、硅酸镁盐(滑石)、云母、碳酸钙、硫酸钡、玻璃珠、玻璃球等。另外,无机填充材料(B)优选含有选自硅酸铝盐、硅酸钙盐中的至少1种作为主要构成成分,更优选含有硅酸铝盐作为主要构成成分。硅酸铝盐在成形时外观也优异,在镀敷工序中使用的蚀刻液中也不溶解,因此容易显示出凹凸,镀敷密贴性优异。这些不仅可以单独仅使用1种,也可以组合使用多种。
为了提高无机填充材料(B)与半芳香族聚酰胺树脂(A)之间的亲和性,无机填充材料(B)优选用有机处理剂或偶联剂处理。或者,优选在熔融复合时与偶联剂并用,作为偶联剂,可以使用硅烷系偶联剂、钛酸盐系偶联剂、铝系偶联剂中的任意种,其中,特别优选氨基硅烷偶联剂、环氧硅烷偶联剂。
作为在本发明的半芳香族聚酰胺树脂组合物的表面实施金属镀敷的方法的一个例子,可举出使蚀刻液与使用半芳香族聚酰胺树脂组合物成形得到的成形体的表面接触,并进行蚀刻(表面粗糙化),在成形体表面上形成凹凸结构,然后在表面上实施金属镀敷的方法。推测通过蚀刻所形成的凹凸显现机械接合效果从而可以得到优异的镀敷粘合性。
本发明中使用的无机填充材料(B)的混合量,相对于半芳香族聚酰胺树脂(A)100质量份,需要为10~200质量份。另外,优选为10~190质量份,更优选为15~180质量份,进一步优选为20~170质量份。无机填充材料(B)的混合量低于上述下限时,由于蚀刻后的凹凸不充分,因此有无法显现出良好的镀敷粘合性的可能性。无机填充材料(B)的混合量超过上述上限时,蚀刻后的凹凸虽然增加,但有导致成形加工性降低的可能性。本发明的半芳香族聚酰胺树脂组合物中,混合量直接作为半芳香族聚酰胺树脂组合物中的含量。
本发明中使用的韧性改良材料(C)不仅可以提高半芳香族聚酰胺树脂组合物的韧性,还可以提高金属镀敷密贴性。作为韧性改良材料,只要是能够提高半芳香族聚酰胺树脂组合物的韧性的材料,就没有特别限定,例如可以举出烯烃系共聚物、弹性体、合成橡胶、天然橡胶。
作为韧性改进材料(C)的一个例子,可列举烯烃系共聚物、离聚物等烯烃系聚合物、苯乙烯系弹性体、聚氨酯系弹性体、氟系弹性体、氯乙烯系弹性体、聚酯系弹性体、聚酰胺系弹性体等弹性体;硫醇橡胶、多硫化橡胶、丙烯酸橡胶、有机硅橡胶、聚醚橡胶、表氯醇橡胶等合成橡胶。另外,从与半芳香族聚酰胺树脂(A)的相容性、耐热性的观点出发,优选烯烃系聚合物、弹性体,更优选烯烃系共聚物、苯乙烯系弹性体。作为烯烃系共聚物,优选(乙烯和/或丙烯)·α-烯烃系共聚物、(乙烯和/或丙烯)·(α,β-不饱和羧酸和/或不饱和羧酸酯)系共聚物。作为苯乙烯系弹性体,优选苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物。这些不仅可以单独仅使用一种,也可以多种组合使用。作为韧性改良材料(C),特别优选使用(乙烯和/或丙烯)·α-烯烃系共聚物、苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物中的至少1种。
本发明中使用的(乙烯和/或丙烯)·α-烯烃系共聚物是使乙烯和/或丙烯与碳原子数4以上的α-烯烃进行共聚而得到的共聚物,作为具有碳原子数4以上的α-烯烃,可列举1-丁烯、1-戊烯、1-己烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯、1-十一碳烯、1-十二碳烯、1-十三碳烯、1-十四碳烯、1-十五碳烯、1-十六碳烯、1-十七碳烯、1-十八碳烯、1-十九碳烯、1-二十碳烯、3-甲基-1-丁烯、4-甲基-1-丁烯、3-甲基-1-戊烯、3-乙基-1-戊烯、4-甲基-1-戊烯、4-甲基-1-己烯、4,4-二甲基-1-己烯、4,4-二甲基-1-戊烯、4-乙基-1-己烯、3-乙基-1-己烯、9-甲基-1-癸烯、11-甲基-1-十二碳烯、12-乙基-1-十四碳烯及它们的组合。此外,可以将1,4-戊二烯、1,4-己二烯、1,5-己二烯、1,4-辛二烯、1,5-辛二烯、1,6-辛二烯、1,7-辛二烯、2-甲基-1,5-己二烯、6-甲基-1,5-庚二烯、7-甲基-1,6-辛二烯、4-亚乙基-8-甲基-1,7-壬二烯、4,8-二甲基-1,4,8-癸三烯(DMDT)、二环戊二烯、环己二烯、二环辛二烯、亚甲基降冰片烯、5-乙烯基降冰片烯、5-亚乙基-2-降冰片烯、5-亚甲基-2-降冰片烯、5-异亚丙基-2-降冰片烯、6-氯甲基-5-异丙烯基-2-降冰片烯、2,3-二异亚丙基-5-降冰片烯、2-亚乙基-3-异亚丙基-5-降冰片烯、2-丙烯基-2,2-降冰片二烯等非共轭二烯的多烯进行共聚。
(乙烯和/或丙烯)·(α,β-不饱和羧酸和/或不饱和羧酸酯)系共聚物是将乙烯和/或丙烯与α,β-不饱和羧酸和/或不饱和羧酸酯单体共聚而得到的聚合物,作为α,β-不饱和羧酸单体,可以举出丙烯酸、甲基丙烯酸,作为α,β-不饱和羧酸酯单体,可列举这些不饱和羧酸的甲酯、乙酯、丙酯、丁酯、戊酯、己酯、庚酯、辛酯、壬酯、癸酯等,或它们的混合物。
离聚物聚合物是烯烃与α,β-不饱和羧酸共聚物的羧基的至少一部分通过金属离子的中和而被离子化而获得的聚合物。作为烯烃,优选乙烯,作为α,β-不饱和羧酸,优选丙烯酸、甲基丙烯酸,但并不限定于这里例示的物质,也可以将不饱和羧酸酯单体共聚。作为金属离子,可列举Li、Na、K、Mg、Ca、Sr、Ba等碱金属、碱土金属,此外可举出Al、Sn、Sb、Ti、Mn、Fe、Ni、Cu、Zn、Cd等。
在本发明中使用的弹性体中,苯乙烯系弹性体是由苯乙烯等芳香族乙烯基化合物系聚合物嵌段和共轭二烯系聚合物嵌段构成的嵌段共聚物,使用具有至少1个芳香族乙烯基化合物系聚合物嵌段和至少1个共轭二烯系聚合物嵌段的嵌段共聚物。此外,在上述嵌段共聚物中,共轭二烯系聚合物嵌段中的不饱和键可以被氢化。
芳香族乙烯基化合物系聚合物嵌段是以源自芳香族乙烯基化合物的结构单元为主而成的聚合物嵌段。作为芳香族乙烯基化合物,可列举苯乙烯、α-甲基苯乙烯、邻甲基苯乙烯、间甲基苯乙烯、对甲基苯乙烯、2,4-二甲基苯乙烯、2,6-二甲基苯乙烯、乙烯基萘、乙烯基蒽、4-丙基苯乙烯、4-环己基苯乙烯、4-十二烷基苯乙烯、2-乙基-4-苄基苯乙烯、4-(苯基丁基)苯乙烯等。此外,芳香族乙烯基化合物系聚合物嵌段可以具有由1种或2种以上的上述单体构成的结构单元,也可以具有由少量的其他不饱和单体构成的结构单元。
共轭二烯聚合物嵌段是由1,3-丁二烯、氯丁二烯、异戊二烯、2,3-二甲基-1,3-丁二烯、1,3-戊二烯、4-甲基-1,3-戊二烯、1,3-己二烯等共轭二烯系化合物的1种或2种以上形成的聚合物嵌段,在经过氢化的芳香族乙烯基化合物/共轭二烯嵌段共聚物中,其共轭二烯系聚合物嵌段中的不饱和键部分的一部分或全部通过氢化而成为饱和键。这里,以共轭二烯作为主体的聚合物嵌段中的分布可以是无规型、锥型、部分嵌段型或它们的任意组合。
芳香族乙烯基化合物·共轭二烯嵌段共聚物及其氢化物的分子结构,可以是直链状、支链状、放射状或其它们的任意组合中的任意种。其中,在本发明的半芳香族聚酰胺树脂组合物中,作为芳香族乙烯基化合物·共轭二烯嵌段共聚物和/或其氢添化物,优选1个芳香族乙烯基化合物聚合物嵌段和1个共轭二烯聚合物嵌段直链状键合而成的二嵌段共聚物;以芳香族乙烯基化合物聚合物嵌段·共轭二烯聚合物嵌段·芳香族乙烯基化合物聚合物嵌段的顺序3个聚合物嵌段直链状键合而成的三嵌段共聚物及它们的氢化物的1种或2种以上,可列举未氢化或氢化苯乙烯·丁二烯共聚物、未氢化或氢化苯乙烯·异戊二烯共聚物、未氢化或氢化苯乙烯·异戊二烯·苯乙烯共聚物、未氢化或氢化苯乙烯·丁二烯·苯乙烯共聚物、未氢化或氢化苯乙烯·异戊二烯·丁二烯·苯乙烯共聚物、未氢化或氢化苯乙烯·乙烯·丁二烯·苯乙烯嵌段共聚物等。
本发明中使用的韧性改良材料(C)优选被羧酸和/或其衍生物改性。通过用这些成分进行改性,可以将具有与半芳香族聚酰胺树脂(A)的亲和性的官能团导入道到分子中,提高与半芳香族聚酰胺树脂(A)的相容性。作为具有与半芳香族聚酰胺树脂(A)的亲和性的官能团,可列举羧酸基、羧酸酐基、羧酸酯基、羧酸金属盐基、羧酸酰亚胺基、羧酸酰胺基、环氧基等。韧性改良材料(C)特别优选为被羧酸和/或其衍生物改性的、(乙烯和/或丙烯)·α-烯烃系共聚物、苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物中的至少1种。
作为可以提高与半芳香族聚酰胺树脂(A)的亲和性的化合物,可列举丙烯酸、甲基丙烯酸、马来酸、富马酸、衣康酸、巴豆酸、甲基马来酸、甲基富马酸、中康酸、柠康酸、戊二酸、顺-4-环己烯-1,2-二羧酸、内双环[2.2.1]-5-庚烯-2,3-二羧酸及这些羧酸的金属盐、马来酸单甲酯、衣康酸单甲酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯、丙烯酸羟乙酯、甲基丙烯酸甲酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸羟乙酯、甲基丙烯酸氨基乙酯、马来酸二甲酯、衣康酸二甲酯、马来酸酐、衣康酸酐、柠康酸酐、内双环-[2.2.1]-5-庚烯-2,3-二羧酸酐、马来酰亚胺、N-乙基马来酰亚胺、N-丁基马来酰亚胺、N-苯基马来酰亚胺、丙烯酰胺、甲基丙烯酰胺、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、乙基丙烯酸缩水甘油酯、衣康酸缩水甘油酯、柠康酸缩水甘油酯等。
本发明中使用的韧性改良材料(C)的混合量,相对于半芳香族聚酰胺(A)100质量份,需要为2~30质量份。另外,优选为2~28质量份,更优选为2~25质量份,进一步优选为3~25质量份。通过使韧性改良材料(C)的混合量在上述范围,除了能够赋予优异的金属镀敷密贴性之外,还可以赋予高拉伸伸长率,可以抑制成形时的裂纹、实际使用时的裂纹。韧性改良材料(C)的混合量低于上述下限时,有金属镀敷密贴性不充分的可能性,另外有产生成形时的裂纹、实际使用时的裂纹的可能性。韧性改良材料(C)的混合量超过上述上限时,作为半芳香族聚酰胺树脂组合物的耐热性、变形受损,有可能发生回流焊接工序中的成形体的变形、在实际使用时的变形。本发明的半芳香族聚酰胺树脂组合物中,混合量直接成为半芳香族聚酰胺树脂组合物中的含量。
本发明的半芳香族聚酰胺树脂组合物,虽然是可以通过如上所述地将无机填充材料(B)以规定的混合量混合至半芳香族聚酰胺树脂(A),可以在蚀刻后的成形体表面形成凹凸,通过机械接合效果提高金属镀敷密贴性的物质,但通过进一步混合韧性改进材料(C)可以表现出更良好的金属镀敷密贴性。推测:通过混合韧性改良材料,在金属镀敷与半芳香族聚酰胺树脂组合物之间的界面处,除了由于凹凸而产生的机械接合效果外,半芳香族聚酰胺树脂组合物的粘性发挥作用,表现出优异的金属镀敷密贴性。
本发明的半芳香族聚酰胺树脂组合物,除了如上所述地将规定量的无机填充材料(B)混合至半芳香族聚酰胺树脂(A)中之外,还以规定量混合韧性改良材料(C),由此可以表现出在仅混合无机填充材料的体系中难以表现出的高拉伸伸长率。
在本发明的半芳香族聚酰胺树脂组合物(C)中,可以在不损害其特性的范围使用以往的聚酰胺树脂组合物中使用的各种添加剂。作为添加剂,可以举出稳定剂、脱模剂、滑动性改良材料、着色剂、增塑剂、结晶成核剂、与半芳香族聚酰胺树脂(A)不同的聚酰胺、聚酰胺以外的热塑性树脂等。这些成分在半芳香族聚酰胺树脂组合物中的可能的混合量如下文中所说明,但这些成分的合计在半芳香族聚酰胺树脂组合物中优选为30质量%以下,更优选为20质量%以下,进一步优选为10质量%以下,特别优选为5质量%以下。
作为稳定剂,可以举出受阻酚系抗氧化剂、硫系抗氧化剂、磷系抗氧化剂等有机系抗氧化剂、热稳定剂、受阻胺系、二苯甲酮系、咪唑系等光稳定剂或紫外线吸收剂、金属钝化剂、铜化合物等。作为铜化合物,可以使用氯化亚铜、溴化亚铜、碘化亚铜、氯化铜、溴化铜、碘化铜、磷酸铜、焦磷酸铜、硫化铜、硝酸铜、乙酸铜等有机羧酸的铜盐等。另外,作为铜化合物以外的构成成分,优选含有卤化碱金属化合物,作为卤化碱金属化合物,可以列举出氯化锂、溴化锂、碘化锂、氟化钠、氯化钠、溴化钠、碘化钠、氟化钾、氯化钾、溴化钾、碘化钾等。这些添加剂不仅可以单独仅使用1种,也可以组合多种使用。稳定剂的添加量只要选择最佳的量即可,相对于100质量份的半芳香族聚酰胺树脂(A),最多可以添加5质量份。
作为脱模剂,可以举出长链脂肪酸或其酯或金属盐、酰胺系化合物、聚乙烯蜡、硅酮、聚环氧乙烷等。作为长链脂肪酸,特别优选碳原子数12以上,例如举出硬脂酸、12-羟基硬脂酸、山嵛酸、褐煤酸等。部分或全部羧酸可以被单二醇或聚二醇酯化,或者也可以形成金属盐。作为酰胺系化合物,可以举出乙烯双对苯二甲酰胺、亚甲基双硬脂酰胺等。这些脱模剂可以单独使用或作为混合物使用。脱模剂的添加量只要选择最佳的量即可,但相对于半芳香族聚酰胺树脂(A)100质量份,最大可以添加5质量份。
在本发明的半芳香族聚酰胺树脂组合物中,也可以将与半芳香族聚酰胺树脂(A)不同组成的聚酰胺进行聚合物共混。虽然与半芳香族聚酰胺树脂(A)不同组成的聚酰胺的添加量只要选择最佳的量即可,但相对于半芳香族聚酰胺树脂(A)100质量份,可以添加最多50质量份。
在本发明的半芳香族聚酰胺树脂组合物中,可以添加聚酰胺以外的热塑性树脂。作为聚酰胺以外的聚合物,可以举出聚苯硫醚(PPS)、液晶聚合物(LCP)、芳纶树脂、聚醚醚酮(PEEK)、聚醚酮(PEK)、聚醚酰亚胺(PEI)、热塑性聚酰亚胺、聚酰胺酰亚胺(PAI)、聚醚酮酮(PEKK)、聚苯醚(PPE)、聚醚砜(PES)、聚砜(PSU)、聚芳酯(PAR)、聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚萘二甲酸乙二醇酯、聚萘二甲酸丁二醇酯、聚碳酸酯(PC)、聚甲醛(POM)、聚丙烯(PP)、聚乙烯(PE)、聚甲基戊烯(TPX)、聚苯乙烯(PS)、聚甲基丙烯酸甲酯、丙烯腈-苯乙烯共聚物(AS)、丙烯腈-丁二烯-苯乙烯共聚物(ABS)。这些热塑性树脂也可以通过熔融混炼以熔融状态进行混合,但也可以将热塑性树脂制成纤维状、粒子状而分散在本发明的聚酰胺树脂组合物中。热塑性树脂的添加量只要选择最佳的量即可,但相对于半芳香族聚酰胺树脂(A)100质量份,最大可以添加50质量份。
本发明的半芳香族聚酰胺树脂组合物中添加芳香族聚酰胺树脂(A)以外的热塑性树脂时,优选共聚有能与聚酰胺反应的反应性基团,作为反应性基团,是能与作为聚酰胺树脂的末端基团的氨基、羧基和主链酰胺基进行反应的基团。具体地,可以例示羧酸基、酸酐基、环氧基、噁唑啉基、氨基、异氰酸酯基等,其中,酸酐基的反应性最优异。
本发明的半芳香族聚酰胺树脂组合物可以通过以往公知的方法混合上述各构成成分来制造。例如,可以在半芳香族聚酰胺树脂(A)的缩聚反应时添加各成分,或可以将半芳香族聚酰胺树脂(A)与其他成分干混,或者使用双螺杆型挤出机将各构成成分熔融混炼的方法。
本发明的半芳香族聚酰胺树脂组合物可以通过注射成形等公知的成形方法制成成形体。使用本发明的半芳香族聚酰胺树脂组合物制造成形体时,注射成形时的模具温度优选为180℃以下,更优选为170℃以下,进一步优选为160℃,特别优选为150℃以下。超过模具温度的上述上限时,有引起成形体残留在模具中等成形不良的可能性。模具温度的下限没有特别限定,但从树脂的流动性、成形体的外观、抑制实际使用环境中的尺寸变化的观点出发,优选为50℃以上,更优选为70℃以上,进一步优选为100℃以上,特别优选为120℃以上。
本发明的半芳香族聚酰胺树脂组合物可以用作在使用其而得到的成形体的表面实施了金属镀敷的金属镀敷成形体。与传统的金属镀敷成形体相比,该金属镀敷成形体的金属镀敷密贴性、低吸水性、耐回流焊接性优异。
作为制造使用了本发明的半芳香族聚酰胺树脂组合物的金属镀敷成形体的方法没有特别限定,可以通过公知的技术制造。作为一个例子,可列举通过使用了铬酸、高锰酸、盐酸等化学蚀刻处理使表面粗化后,利用粗化表面用依次进行中和、施加催化剂、活性化、无电解镀敷、酸活性、电镀等工序的催化剂·促进剂法;通过省略该催化剂·促进剂法中的无电解镀敷工序的直接镀敷法等实施金属镀敷的方法;通过紫外线、具有特定波长的激光对表面进行改性,然后利用改性表面,依次进行施加催化剂、活性化、无电解镀敷、酸活性、电镀等工序的催化剂·促进剂法;通过省略该催化剂·促进剂法中的无电解镀敷工序的直接镀敷法等实施金属镀敷的方法。此外,蚀刻及金属镀敷可以对镀敷用成形体表面整体或其一部分进行。
使用了本发明的半芳香族聚酰胺树脂组合物的金属镀敷成形体的金属镀敷的厚度,只要选择最佳厚度即可,但优选0.5~200μm,更优选1~150μm。
使用了本发明的半芳香族聚酰胺树脂组合物的金属镀敷成形体,由于在半芳香族聚酰胺树脂组合物中混合的无机填充材料、韧性改良材料,而具有优异的金属密贴性。
使用了本发明的半芳香族聚酰胺树脂组合物的金属镀敷成形体的金属镀敷剥离强度,通过以下实施例的项目中说明的方法进行测定。金属镀敷剥离强度是涉及本发明的半芳香族聚酰胺树脂组合物的良好镀敷性的项目,金属镀敷剥离强度需要为4.0N/cm以上,优选为5.0N/cm以上。另外,要抑制使用环境下的金属镀敷的翘起、剥离这样密贴不良的发生,具有更高的金属镀敷剥离强度是有利的,更优选为6.0N/cm以上。本发明中可以实现这种镀金属剥离强度。金属镀层剥离强度更优选为6.5N/cm以上。金属镀敷剥离强度低于上述下限时,半芳香族聚酰胺树脂组合物与金属镀敷的密贴性低,有产生金属镀敷的翘起或剥离的可能性。
使用了本发明的半芳香族聚酰胺树脂组合物的金属镀敷成形体的拉伸伸长率,通过下述实施例的项目中说明的方法进行测定。拉伸伸长率是与本发明的半芳香族聚酰胺树脂组合物的成形加工性、产品实际使用时的耐久性有关的项目,拉伸伸长率需要为1.5%以上,优选为1.7%以上。拉伸伸长率低于上述下限时,有产生成形时的裂纹或实际使用时的裂纹的可能性。
使用了本发明的半芳香族聚酰胺树脂组合物的金属镀敷成形体,发挥良好的金属镀敷密贴性,可以用于汽车部件、电气电子部件、办公自动化机器部件、电磁波屏蔽部件等各种用途。
实施例
在下文中,将通过实施例更具体地对本发明进行说明,但本发明不限于这些实施例。需要说明的是,实施例中记载的测定值是通过以下方法测定的测定值。
(1)末端氨基浓度(AEG)、末端羧基浓度(CEG)
将半芳香族聚酰胺树脂(A)溶于氘代氯仿(CDCl3)/六氟异丙醇(HFIP)=1/1(体积比)的溶剂中,滴下氘代甲酸之后,用1H-NMR测定各末端基浓度。
(2)相对粘度(RV)
将0.25g半芳族聚酰胺树脂溶解在25ml的96%的硫酸中,在20℃下使用奥氏粘度计进行测定。
(3)熔点(Tm)
将105℃下减压干燥15小时的半芳香族聚酰胺树脂于铝制盘(SII NanoTechnology公司制造,型号170421S)中计量10mg,用铝制盖(SII Nano Technology公司制造,型号170420)制成密封状态,制备测定试样后,用高灵敏度型差示式扫描量热仪DSC7020(SII Nano Technology公司制造)从室温以20℃/分钟升温,在350℃保持3分钟后取出测定试样盘,浸入液氮中,使之骤冷。然后,从液氮中取出样品,在室温下放置30分钟后,再次使用高灵敏度型差示扫描量热计DSC7020(SII NanoTechnology公司制造),从室温开始以20℃/分钟升温,在350℃下保持3分钟。将升温时的熔解引起的吸热的峰值温度作为熔点(Tm)。
(4)80℃、95%RH平衡吸水率
使用东芝机械制造的注射成形机EC-100,将机筒温度设定为树脂的熔点+20℃,将模具温度设定为140℃,注射成形出纵100mm、横100mm、厚1mm的平板,制作评价用试验片。将该试验片在150℃的气氛下退火处理2小时后,测定质量,将此时的质量作为干燥时的质量。进一步,将退火处理后的试验片在85℃、95%RH(相对湿度)的气氛下静置1000小时,之后测定质量,将此时的质量作为饱和吸水时的质量。根据用上述方法测定的饱和吸水时和干燥时的质量,由以下的式求出80℃、95%RH平衡吸水率。
80℃、95%RH平衡吸水率(%)={(饱和吸水时的质量-干燥时的质量)/干燥时的质量}×100
(5)拉伸伸长率
使用东芝机械制造的注射成形机EC-100,将机筒温度设定为树脂的熔点+20℃,将模具温度设定为140℃,依据ISO 294-1,制备多目的试验片(ISO3167)。使用制备的试验片,按照ISO 527-1,2进行拉伸伸长率评价。
(6)金属镀敷剥离强度
使用东芝机械制造的注射成形机EC-100,将机筒温度设置为树脂的熔点+20℃,将模具温度设置为140℃,注射成形出纵100mm、横100mm、厚2mm的平板,制作评价用试验片。将得到的试验片用异丙醇擦拭后,使用50g/l的OPC-250清洁剂(クリ一ナ一)(奥野制药株式会社制)在60℃下脱脂处理3分钟。然后,将试验片在由400g/l的铬酸、200ml/l的浓硫酸和0.3g/l的トツプシヤツト(奥野制药株式会社制)构成的70℃的铬酸溶液中浸渍5分钟,进行表面处理。将进行了表面处理的试验片在室温下用38%盐酸的5%水溶液实施3分钟酸洗,然后在调整至45℃的由200ml/l的B-200中和剂(ニユ一トライザ一)(奥野制药株式会社制)构成的处理液中浸渍5分钟。接着,将其在由调整为25℃的锡-钯络盐水溶液(A30催化剂,奥野制药株式会社制)、盐酸与水(体积比=1∶1∶5)构成的处理液中浸渍4分钟(催化)。然后,在调整为50℃的38%盐酸的10%水溶液中浸渍4分钟后(促进),在由调整为40℃的TMP化学镍A液、B液(奥野制药株式会社制)和水(体积比=1∶1∶4)构成的无电解镍镀敷液中浸渍10分钟,在试验片表面形成约1μm的镍镀敷层,进一步实施电解铜镀敷,形成铜镀敷层。从得到的金属镀敷试验片切出纵100mm、横10mm、厚2mm的条状试验片,作为剥离强度评价试验片。使用制作的剥离强度评价试验片,按照JIS H8630 90度剥离强度试验方法测定金属镀敷剥离强度。
(7)金属镀敷外观
使用东芝机械制造的注射成形机EC-100,将机筒温度设定为树脂的熔点+20℃,将模具温度设定为140℃,注射成形出纵100mm、横100mm、厚2mm的平板,制作评价用试验片。将得到的试验片用异丙醇擦拭后,使用50g/l的OPC-250清洁剂(奥野制药株式会社制)在60℃下脱脂处理3分钟。然后,将试验片在由400g/l的铬酸、200ml/l的浓硫酸和0.3g/l的トツプシヤツト(奥野制药株式会社制)构成的70℃的铬酸溶液中浸渍5分钟,进行表面处理。将进行了表面处理的试验片在室温下用38%盐酸的5%水溶液实施3分钟酸洗,然后在调整至45℃的由200ml/l的B-200中和剂(奥野制药株式会社制)构成的处理液中浸渍5分钟。接着,将其在由调整为25℃的锡-钯络盐水溶液(A30催化剂,奥野制药株式会社制)、盐酸、水(体积比=1∶1∶5)构成的处理液中浸渍4分钟(催化)。然后,在调整为50℃的38%盐酸的10%水溶液中浸渍4分钟后(促进),在调整为40℃的由TMP化学镍A液、B液(奥野制药株式会社制)和水(体积比=1∶1∶4)构成的无电解镀镍液中浸渍10分钟,在试验片表面形成约1μm的镍镀敷层,进一步实施电解铜镀敷,形成铜镀敷层。观察得到的金属镀敷试验片的外观,通过金属镀敷有无翘起来评价外观。
○:无金属镀敷的翘起
×:有金属镀敷的翘起
(8)耐回流焊接性
使用东芝机械制造的注射成形机EC-100,将机筒温度设定为树脂的熔点+20℃,将模具温度设定为140℃,注射成形出长127mm、宽12.6mm、厚0.8mm的UL燃烧试验用试样,制作试验片。试验片在85℃、85%RH(相对湿度)的气氛中放置72小时。试验片在空气回流炉中(Eitec制AIS-20-82C),用60秒从室温升温至150℃,进行预热后,以0.5℃/分钟的升温速度实施预热至190℃。然后,以100℃/分钟的速度升温至规定的设定温度,在规定的温度下保持10秒后,进行冷却。使设定温度从240℃以5℃的间隔增加,将没有发生表面膨胀、变形的最高设定温度作为回流耐热温度,作为焊接耐热性的指标使用。
○:回流耐热温度为260℃以上
×:回流耐热温度低于260℃
在本实施例中,作为半芳香族聚酰胺树脂(A),使用通过以下方法合成的树脂或市售品。表1显示了各半芳族聚酰胺树脂(A)的物性。
[表1]
<合成例1;半芳香族聚酰胺树脂(A1)>
将8.55kg 1,6-六亚甲基二胺、12.25kg对苯二甲酸、8.00kg 11-氨基十一烷酸、9g作为催化剂的次亚磷酸钠、140g作为末端调节剂的乙酸和16.20kg离子交换水装入到50升高压釜中,用N2从常压加压至0.05MPa,放压,恢复到常压。这个操作进行3次,进行N2置换后,在搅拌下,在135℃、0.3MPa下使其均匀溶解。
然后,用送液泵连续供给溶解液,用加热配管升温至240℃,加热1小时。然后,向加压反应釜中供给反应混合物,加热至290℃,使一部分水馏出,以便釜内压维持在3MPa,得到低级缩合物(日语:低次合物)。然后,将该低级缩合物以维持熔融的状态直接供给到双螺杆挤出机(螺杆直径37mm、L/D=60),将树脂温度定为335℃,一边从3处的出口排出水,一边在熔融下进行缩聚,得到半芳香族聚酰胺树脂(A1)。所得到的半芳香族聚酰胺树脂(A1)由65.1摩尔%的由1,6-六亚甲基二胺和对苯二甲酸构成的结构单元、34.9摩尔%的由11-氨基十一烷酸构成的结构单元构成,相对粘度为2.1,熔点为314℃,AEG=30eq/ton、CEG=140eq/ton。聚酰胺树脂的构成单体比率与AEG及CEG测定同样地通过1H-NMR确认。
<合成例2;半芳香族聚酰胺树脂(A2)>
按照日本国专利特开平7-228689号公报的实施例1中记载的方法,合成了由对苯二甲酸单元、1,9-壬二胺单元和2-甲基-1,8-辛二胺单元(1,9-壬二胺单元:2-甲基-1,8-辛二胺单元的摩尔比为85:15)构成的半芳香族聚酰胺树脂(封端剂使用苯甲酸)。所得到的半芳香族聚酰胺树脂(A2)由85.2%摩尔%的由1,9-壬二胺单元和对苯二甲酸构成的结构单元、14.8摩尔%的由2-甲基-1,8-辛二胺单元和对苯二甲酸构成的结构单元构成,相对粘度为2.1,熔点为286℃,AEG=13eq/ton、CEG=50eq/ton。聚酰胺树脂的构成单体比率与AEG及CEG测定同样地通过1H-NMR确认。
本实施例是使用如以下所例示地制作的半芳香族聚酰胺树脂进行的。
以表2和3中记载的成分和质量比例(质量份),使用Coperion株式会社制造的双螺杆挤出机STS-35,在各聚酰胺原料的熔点+20℃下熔融混炼,得到实施例1~11、比较例1~5的半芳香族聚酰胺树脂组合物。制作半芳香族聚酰胺树脂组合物时所用的原料如下所示。作为其他添加剂使用的脱模剂和稳定剂以1∶5的质量比例使用。
半芳香族聚酰胺树脂(A1):根据上述的合成例1制作的半芳香族聚酰胺树脂
半芳香族聚酰胺树脂(A2):根据上述的合成例2制作的半芳香族聚酰胺树脂
半芳香族聚酰胺树脂(A3):PA6T/6(BASF株式会社制Ultramide(R)KR4351、Tm=290℃)
无机填充材料(B1):煅烧高岭土(BASF株式会社制造、Translink(R)445、有表面处理、平均粒径1.4μm)
无机填充材料(B2):煅烧高岭土(BASF株式会社制造、Satintone(R)5HB、有表面处理、平均粒径0.8μm)
无机填充材料(B3):纤维状硅灰石(NYCO株式会社制造、NYGLOS(R)8、有表面处理)
韧性改良材料(C1):马来酸酐改性的苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物(旭化成株式会社制造,Tuftec(R)M1943)
韧性改良材料(C2):马来酸酐改性的乙烯-丁烯共聚物(三井化学株式会社制造、Tafmer(R)MH7020)
韧性改良材料(C3):马来酸酐改性丙烯-丁烯共聚物(三井化学株式会社制造,Tafmer(R)MP0620)
韧性改良材料(C4):乙烯-丙烯酸酯-马来酸酐共聚物(Arkema株式会社,ボンダィン(R)AX-8390)
脱模剂:硬脂酸镁
稳定剂:季戊四醇四[3-(3,5-二叔丁基-4-羟基苯基)丙酸酯](Chiba SpecialityChemicals公司制造Irganox 1010)
[表2]
[表3]
<实施例1~11、比较例1~5>
由表2可知,实施例1~11表现出优异的拉伸伸长率、金属镀敷剥离强度、金属镀敷外观的同时,还具有耐回流焊接性,具有优异的特性。此外,在实施例1~7、9中显示出特别优异的金属镀敷剥离强度,可知具有优异的特性。另一方面,由表3可知,比较例1、2中,金属镀敷外观、耐回流焊接性虽然良好,但由于没有混合韧性改良材料(C),因此拉伸伸长率低,金属镀敷剥离强度也比实施例低,抑制使用环境下的镀敷密贴不良并不充分。在比较例3中,虽然拉伸伸长率、耐回流焊接性良好,但由于没有混合无机填充材料(B),所以金属镀敷剥离强度、金属镀敷外观较差。在比较例4中,使用了与实施例1~10不同的半芳香族聚酰胺(PA9T/M8T),虽然耐回流焊接性良好,但拉伸伸长率低,金属镀敷剥离强度也比实施例低,抑制使用环境下的镀敷密贴不良并不充分。比较例5中使用与实施例1~11不同的半芳香族聚酰胺(PA6T/6),拉伸伸长率低,金属镀敷层剥离强度也比实施例低,除了抑制使用环境下的镀敷密贴不良并不充分之外,由于80℃、95%RH饱和吸水率高,因此耐回流焊接性较差。
产业上的可利用性
本发明的半芳香族聚酰胺树脂组合物除了半芳香族聚酰胺树脂的组成以外,还通过混合无机填充材料、韧性改良材料,表现出良好的金属镀敷密贴性、镀敷外观,与此同时也可以满足耐回流焊接性,可以在工业上有利地制造需要金属镀敷的成形品。
Claims (6)
1.一种半芳香族聚酰胺树脂组合物,相对于半芳香族聚酰胺A 100质量份,含有无机填充材料B 10~200质量份以及韧性改良材料C 2~30质量份,所述半芳香族聚酰胺树脂A满足下述(a)、(b),
(a)通过差示扫描量热法DSC测得的熔点Tm为280℃以上,
(b)80℃、95%RH平衡吸水率为3.5%以下。
2.根据权利要求1所述的半芳香族聚酰胺树脂组合物,韧性改良材料C为选自烯烃系共聚物及苯乙烯系弹性体中的至少一种。
3.根据权利要求2所述的半芳香族聚酰胺树脂组合物,烯烃系共聚物是选自(乙烯和/或丙烯)·α-烯烃系共聚物以及(乙烯和/或丙烯)·(α,β-不饱和羧酸和/或不饱和羧酸酯)系共聚物中的至少一种。
4.根据权利要求2或3所述的半芳香族聚酰胺树脂组合物,苯乙烯系弹性体为苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物。
5.根据权利要求1~4中任一项所述的半芳香族聚酰胺树脂组合物,无机填充材料B含有硅酸铝盐、硅酸钙盐。
6.一种金属镀敷成形体,使用了权利要求1~5中任一项所述的半芳香族聚酰胺树脂组合物。
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KR20220108044A (ko) | 2022-08-02 |
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