CN100540297C - 抗冲改性聚酰胺膜 - Google Patents
抗冲改性聚酰胺膜 Download PDFInfo
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- CN100540297C CN100540297C CNB200480023871XA CN200480023871A CN100540297C CN 100540297 C CN100540297 C CN 100540297C CN B200480023871X A CNB200480023871X A CN B200480023871XA CN 200480023871 A CN200480023871 A CN 200480023871A CN 100540297 C CN100540297 C CN 100540297C
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Abstract
本发明提供一种膜，其包含作为底层的：(1)包含芳族聚酰胺和抗冲改性剂的至少一层L1，和，任选的(2)包含脂族聚酰胺的至少一层L2。
Description
引用相关申请
本申请要求享有在2003年8月19日提交的美国临时申请60/496,011的优先权，通过引用将该临时申请并入本文。
技术领域
本发明涉及由抗冲改性聚酰胺制成的膜。根据本发明的膜包含作为底层(solelayer)的(1)包含芳族聚酰胺和抗冲改性剂的至少一层L1和任选的(2)包含脂族聚酰胺的至少一层L2。
本发明的其它优点和其它特征部分将在下面的说明中阐明，部分将在本领域普通技术人员阅读下文时变得明了，或者可以从本发明的实施中了解。本发明的优点可以如在所附权利要求中具体指出的那样实现和获得。应该认识到，本发明能够有其它的和不同的实施方案，并且它的一些细节能够在多个明显的方面进行修改，所有的这些均不会偏离本发明。说明书在本质上将被认为是说明性的而不是限制性的。
背景技术
聚酰胺膜例如PA6、66、11、12等是已知的并且用于各种应用中。例如，聚酰胺膜用来提供化学、水和燃料阻隔性，或作为电气应用中的绝缘元件。
但是，仍需要改善聚酰胺膜在例如机械性能、耐水性、耐其它溶剂和化学物质性、电绝缘特性等方面的性能。
发明内容
本发明提供一种膜，该膜包含作为底层的(1)包含芳族聚酰胺和抗冲改性剂的至少一层L1和任选的(2)包含脂族聚酰胺的至少一层L2。在优选实施方案中，L1是膜的底层。在另一个优选实施方案中，层L1和L2相互直接接触并且是包括在膜中的底层。在另一个优选实施方案中，膜包括作为底层的三个邻接层，次序为L1/L2/L1。在另一个优选实施方案中，膜包括作为底层的两个或更多邻接L1层。在另一个优选实施方案中，膜包括作为底层的次序为〔(L1)n/(L2)m〕x的任意数量的邻接层，其中x是等于或大于1的任意整数，n是等于或大于1的任意整数，m是任意整数(例如0、1、2等)。在另一个优选实施方案中，膜不含有氟聚合物层。当本发明膜是多层结构时，L1和L2层的每一层可以相互相同或不同。
可以以任意所需的方法由指定材料来制造本发明的膜从而产生层L1和L2，例如通过挤出，这种技术对本领域技术人员来说是公知的。本发明膜的大小、形状、厚度、表面结构等没有任何限制。
附图说明
图1A和图1B是根据本发明用于挤出膜的挤出装置的图解。
具体实施方式
对于三层或更多层的多层结构，术语“内层”理解为膜的最内层。术语“外层”理解为膜的最外层；即，没有其它膜层直接邻接在该外层的外部。多层膜结构具有两个外层。当膜由一层构成时，它被称为“单层”。
聚酰胺
一般说来，聚酰胺是含有重复酰胺(CONH)官能团的聚合物。通常，通过使二胺和二酸单体单元(例如尼龙6，6)反应或者通过聚合氨基羧酸或己内酰胺(例如尼龙6)来形成聚酰胺。聚酰胺是众所周知的材料。本文中有用的聚酰胺包括在美国专利6,531,529、6,359,055、5,665,815、5,436,294、5,447,980、RE34,447、6,524,671(DuPont)、6,306,951(BP Corp.)和5,416,189中所描述的那些以及由Solvay AdvancedPolymers销售的商标名为
和
的那些。本发明涉及芳族和脂族聚酰胺。对由缩聚得到的聚酰胺而言，芳族重复单元的芳香性可以来自的二酸和/或来自二胺。
聚酰胺组合物L1
可用于本文的膜的L1聚酰胺组合物包含芳族聚酰胺和抗冲改性剂。
芳族聚酰胺
芳族聚酰胺是包含50mol％以上“1型”重复单元的聚合物，基于聚合物中100mol％的重复单元。在聚合物链中，1型重复单元具有至少一个CONH基团。另外，1型重复单元的特征在于其至少30mol％包含芳基。因此，基于聚合物中100mol％重复单元，本文中在芳族聚酰胺中含芳基重复单元的最小含量超过15mol％。优选地，基于100mol％的组成聚酰胺的单体，本发明的芳族聚酰胺包含至少20mol％的包含芳基的单体。虽然没有要求，但是这种芳基通常源于二酸单体，并且包括对苯二酸、间苯二酸、邻苯二酸等。在优选实施方案中，基于100mol％的组成聚酰胺的单体，芳族聚酰胺包含至少30mol％的包含芳基的单体，包括35、40、45、50、55、60、65、70、75、80、85等mol％。
一类优选的芳族聚酰胺是PMXDA，即包含50mol％以上的通过至少一种脂族二酸和间苯二甲撑二胺之间缩聚反应形成的重复单元的芳族聚酰胺。
脂族二酸尤其可以是己二酸。
适当的PMXDA尤其可以从Solvay Advanced Polymers以
PMXDA获得。
另一类优选的芳族聚酰胺是聚邻苯二酰胺，即包含50mol％以上的通过至少一种邻苯二甲酸和至少一种脂族二胺之间缩聚反应形成的重复单元的芳族聚酰胺。
脂族二胺可以特别地是六亚甲基二胺、壬二胺、2-甲基-1，5戊二胺和1，4-二氨基丁烷。
适当的聚苯二酰胺尤其可以从Solvay Advanced Polymers，L.L.C以
获得。
在聚苯二酰胺中，优选聚对苯二酰胺。聚对苯二酰胺定义为包含超过50mol％的通过对苯二酸与至少一种二胺之间缩聚反应形成的重复单元的芳族聚酰胺。
一类优选的聚对苯二酰胺是基本由通过对苯二酸与至少一种脂族二胺之间缩聚反应形成的重复单元构成的聚对苯二酰胺。在这类聚对苯二酰胺中，脂族二胺优选包含3-9个碳原子，并且非常优选它包含6个碳原子。包含6个碳原子的脂族二胺的实例是六亚甲基二胺。
第二类优选聚对苯二酰胺是基本由通过对苯二酸、间苯二酸与至少一种脂族二胺之间缩聚反应形成的重复单元构成的聚对苯二酰胺。在该实施方案中，对苯二酸和间苯二酸的摩尔比可以是50-80(包括55、60、65、70和75)的对苯二酸和10-40(包括15、20、25和35)的间苯二酸。在另一个实施方案中，摩尔比可以是35-65的对苯二酸和不超过20的间苯二酸。
第三类优选聚对苯二酰胺是基本由通过对苯二酸、至少一种脂族二酸与至少一种脂族二胺之间缩聚反应形成的重复单元构成的聚对苯二酰胺。在该实施方案中，对苯二酸和脂族二酸的摩尔比可以是50-80(包括55、60、65、70和75)的对苯二酸和不超过25(包括5、10、15和20)的脂族二酸。在另一个实施方案中，摩尔比可以是35-65的对苯二酸和30-60的脂族二酸。
第四类优选聚对苯二酰胺是基本由通过对苯二酸、间苯二酸、至少一种脂族二酸与至少一种脂族二胺之间缩聚反应形成的重复单元构成的聚对苯二酰胺。在该实施方案中，对苯二酸和脂族二酸的摩尔比可以是50-80(包括55、60、65、70和75)的对苯二酸、10-40(包括15、20、25和35)的间苯二酸和不超过25(包括5、10、15和20)的脂族二酸。在另一个实施方案中，摩尔比可以是35-65的对苯二酸、不超过20的间苯二酸和30-60的脂族二酸。
可用于本文中的另一优选芳族聚酰胺是由对苯二酸、己二酸、任选的间苯二酸、和六亚甲基二胺制成的芳族聚酰胺。
在另一个优选实施方案中，芳族聚酰胺是具有至少50mol％包括至多100mol％重复单元的聚酰胺，所述重复单元通过对苯二酸、间苯二酸、己二酸与至少一种二胺优选脂族二胺之间的缩聚反应获得。在该类聚酰胺中，对苯二酸/间苯二酸/己二酸的摩尔比可以是50-80/10-40/不超过25。在另一个实施方案中，对苯二酸/间苯二酸/己二酸的摩尔比可以是35-65/不超过20/30-60。在优选实施方案中，这些酸混合物的二胺组分是HMDA。
在本发明的某些实施方案中，用于形成聚苯二酰胺的二羧酸组分中芳族二羧基的摩尔比为从至少约50mol％芳基到约100mol％芳基。在本发明的优选实施方案中，聚苯二酰胺聚合物包含约50mol％-约95mol％六亚甲基对苯二酰胺单元、约25mol％-约0mol％六亚甲基间苯二酰胺单元和约50mol％-约5mol％己二酰己二胺单元。另一种有用的芳族聚酰胺是由苯二酸、间苯二酸和脂族胺例如HMDA制成的聚酰胺，例如利用70/30比例的TA/IA。特别适用于本发明的聚苯二酰胺可以从Solvay AdvancedPolymers，LLC以
A-1000、A-4000、A-5000和A-6000聚苯二酰胺获得。在先前引用的Poppe等人的美国专利No.5,436,294、5,447,980和Re34,447中公开了本发明适用的聚苯二酰胺。
当然，可以在聚酰胺组合物L1中使用一种以上的芳族聚酰胺。
抗冲改性剂
可用于本文的抗冲改性剂没有具体限制，只要它们为本发明L1层的芳族聚酰胺组分提供有用的性能即可，例如在屈服和断裂时具有足够的拉伸伸长率。例如，具有低于0℃玻璃化转变温度的任意橡胶态低模量官能化聚烯烃抗冲改性剂适合于本发明，包括在U.S.5,436,294和5,447,980中公开的官能化抗冲改性剂。有用的抗冲改性剂包括聚烯烃，优选官能化聚烯烃，尤其是诸如SEBS和EPDM的弹性体。
有用的官能化聚烯烃抗冲改性剂可以从市场上购得，包括可以EXXELORTM PO得到的马来酸聚丙烯和乙烯-丙烯共聚物以及包含约0.6wt％琥珀酐侧基的马来酸酐官能化乙烯-丙烯共聚物橡胶，例如Exxon Mobil化学公司的
RTM.VA1801；可以
得到的丙烯酸酯改性的聚乙烯，例如
9920，来自DuPont公司的甲基丙烯酸改性的聚乙烯；和例如
1410XT，来自Dow化学公司的丙烯酸改性的聚乙烯；马来酸酐改性的苯乙烯-乙烯-丁烯-苯乙烯(SEBS)嵌段共聚物，例如
FG1901X，来自Kraton Polymers的用约2wt％的马来酸酐接枝的SEBS；马来酸酐官能化乙烯-丙烯-二烯单体(EPDM)三元共聚物橡胶，例如
498，来自Crompton Corporation的1％马来酸酐官能化EPDM。本发明的膜并不限于仅仅由这些抗冲改性剂形成的那些。在抗冲改性剂上的适当官能团包括能够与聚酰胺端基反应从而为高温基体提供增强的粘合性的任意化学基团。
也可用于实施本发明的其它官能化抗冲改性剂包括乙烯-高级α-烯烃聚合物和乙烯-高级α-烯烃-二烯聚合物，这些聚合物通过接枝或者与合适的活性羧酸或它们的衍生物例如丙烯酸、甲基丙烯酸、马来酸酐或它们的酯类共聚而提供有活性官能度，并且根据ASTM D-638测定具有至多约50,000psi的拉伸模量。适合的高级α-烯烃包括C3-C8α-烯烃，例如丙烯、丁烯-1、己烯-1和苯乙烯。作为替代方案，具有包含这种单元的结构的共聚物还可以通过聚合1-3种二烯单体的适当均聚物和共聚物的氢化来获得。例如，容易获得具有不同水平的乙烯单元侧基的聚丁二烯，可以将它们氢化以提供乙烯-丁烯共聚物结构。同样，可以采用聚异戊二烯的氢化来提供相当的乙烯-异丁烯共聚物。可用于本发明的官能化聚烯烃包括具有约0.5-约200g/10min的熔融指数的那些官能化聚烯烃。
用于制备乙烯-α-烯烃-二烯三元共聚物的适当二烯是具有4-约24个碳原子的非共轭二烯，其实例包括1，4-己二烯、二环戊二烯和亚烷基降冰片烯例如5-亚乙基-2-降冰片烯。乙烯-高级α-烯烃共聚物橡胶中乙烯单元和高级α-烯烃单元的摩尔分数通常为约40∶60-约95∶5。具有约50-约95mol％乙烯单元以及约5-约50mol％丙烯单元的乙烯-丙烯共聚物包括在这些物质中。在包含聚合二烯单体的三元共聚物中，二烯单元含量可以至高达约10mol％，在某些实施方案中为约1-约5mol％。包含两个或多个聚合物嵌段的相应嵌段共聚物也适合，每一个聚合物嵌段均由选自乙烯和高级α-烯烃的一种或多种单体构成。官能化聚烯烃通常还包含约0.1-约10wt％的官能团。
可用于本文的其它抗冲改性剂包括U.S.6,765,062(Ciba Specialty ChemicalsCorporation)和EP 901507B1(DuPont)中描述的那些。
可用于本文的其它抗冲改性剂还包括由Rohm&Haas销售的名为
抗冲改性剂的丙烯酸抗冲改性剂。
在组合物L1中存在的抗冲改性剂的量没有限制并且优选是足够的量从而赋予足够的拉伸屈服和断裂伸长率。通常，基于组合物L1的总重量，聚酰胺组合物L1将包含约2wt％-约40wt％的抗冲改性剂，例如包括5、10、15、20、25、30和35wt％。但是，抗冲改性剂的含量可以少至例如0.1wt％。
抗冲改性剂和芳族聚酰胺可以以任意方式混合在一起，并且混合可以在例如挤出之前发生，或者可以在挤出机中混合材料。
当然，可以在聚酰胺组合物L1中使用一种以上的抗冲改性剂。
聚酰胺组合物L2
可用于本文的聚酰胺组合物L2形成本发明膜的任选层并且包含脂族聚酰胺。脂族聚酰胺是包含超过50mol％“2型”重复单元的聚合物，基于聚合物中100mol％的重复单元。2型重复单元在聚合物链中具有至少一个CONH基团。另外，2型重复单元的特征在于其30mol％以下包含芳基。因此，基于聚合物中100mol％的重复单元，本文中在脂族聚酰胺中含芳基重复单元的最大含量少于15mol％。优选地，基于100mol％的组成聚酰胺的单体，脂族聚酰胺包含超过85mol％例如90mol％等的包含脂基并且不含芳基的单体。虽然没有要求，但是这种脂基可源于二胺单体，并且包括包含4-12个碳原子的脂族二胺，例如六亚甲基二胺(HMDA)、壬二胺、2-甲基-1，5戊二胺和1，4-二氨基丁烷等。脂族单元的一种有用的二酸源是己二酸。本发明脂族L2聚酰胺的可用实例包括脂族尼龙(例如PA6、PA6，6、PA6，12、PA4，6、PA11、PA12等)。
当然，可以在聚酰胺组合物L2中使用一种以上的脂族聚酰胺。另外，可以根据需要在聚酰胺组合物L2中使用上述抗冲改性剂。
添加剂
聚酰胺组合物L1和L2可以各自独立地任选地还含有一种或多种添加剂。有用的添加剂包括例如有助于挤出的外部润滑剂，例如PTFE或低密度聚乙烯(LDPE)。适合的粉状PTFE包括可得自Solvay Solexis的
F5A。
另一种有用的添加剂是热稳定剂。适合的热稳定剂包括含铜稳定剂，该稳定剂包含可溶于聚酰胺和碱金属卤化物中的铜化合物。更具体地，在某些实施方案中，稳定剂包含铜(I)盐例如乙酸亚铜、硬脂酸亚铜、亚铜有机络合物例如乙酰丙酮化铜、卤化亚铜等以及碱金属卤化物。在本发明的某些实施方案中，稳定剂包含选自碘化铜和溴化铜的卤化铜以及选自锂、钠和钾的碘化物和溴化物的碱金属卤化物。也可以使用包含卤化铜(I)、碱金属卤化物和磷化合物的配方来改善由聚邻苯二酰胺组合物形成的膜在长期暴露于高达约140℃温度期间的稳定性。使用的稳定剂的量优选足以提供约50ppm-约1000ppm水平的铜。本发明的优选组合物包含重量比为约2.5-约10的碱金属卤化物和卤化铜(I)，最优选约8-约10。通常，稳定化的聚酰胺组合物中铜和碱金属卤化物的组合重量为约0.01wt％-约2.5wt％。在用于形成根据本发明膜的某些其它稳定化聚酰胺组合物中，稳定剂的含量为约0.1wt％-约1.5wt％。
根据本发明聚酰胺组合物的特别适合的稳定剂包含碘化钾和碘化亚铜混合物与硬脂酸镁粘合剂重量比为10∶1的小球。碘化钾/碘化亚铜热稳定剂提供保护以防止长期热老化，例如暴露于汽车引擎罩下的温度下时。
另一种有用的添加剂是填料例如补强填料或结构纤维。可用于形成填充制品和复合材料产品的结构纤维包括玻璃纤维、碳或石墨纤维和由碳化硅、氧化铝、氧化钛、硼等形成的纤维以及由高温工程树脂例如聚(苯并噻唑)、聚(苯并咪唑)、多芳基化合物、聚(苯并噁唑)、芳族聚酰胺、聚芳醚等形成的纤维，并可以包括包含两种或更多这种纤维的混合物。可用于本文的适当纤维包括玻璃纤维、碳纤维和芳族聚酰胺纤维例如由DuPont公司销售的商品名为
的纤维。
另一种有用的添加剂是抗氧化剂。有用的抗氧化剂包括Nauguard 445、酚(例如来自Ciba的Irganox 1010、Irganox 1098)、亚磷酸盐、亚膦酸盐(例如来自Ciba的Irgafos 168、来自Clariant或Ciba的P-EPQ)、硫代增效剂(例如来自Great Lakes的Lowinox DSTDP)、受阻胺稳定剂(例如来自Ciba的Chimasorb 944)、羟胺、苯并呋喃酮(benzofuranone)衍生物、丙烯酰改性酚等。
也可用于根据本发明聚酰胺组合物中的其它填料包括抗静电添加剂例如碳粉、多壁碳纳米管和单壁纳米管以及薄片、球形和纤维状颗粒填料增强体和成核剂例如滑石、云母、二氧化钛、钛酸钾、二氧化硅、高岭土、白垩、氧化铝、矿物填料等。填料和结构纤维可以单独使用或任意组合使用。
另外的有用添加剂包括但不限于颜料、染料、阻燃剂等，包括那些常用于树脂技术中的添加剂。添加剂可以根据需要单独使用或任意结合使用。对于具体的应用，它还可以有益地包括增塑剂、润滑剂和脱模剂以及热、氧化和光稳定剂等。对于本领域普通技术人员所设想的具体用途，根据本公开内容可以确定这些添加剂的含量。
方法
可以通过本领域已知的或以后开发的任意技术来制作本发明的膜，具体包括挤出法。在这点上，本领域普通技术人员能够根据本公开内容利用聚酰胺组合物L1和L2来形成本文所描述的本发明膜。
本发明膜的物理尺寸没有限制。单层膜或多层膜的优选厚度是5微米-1000微米(0.05-1mm)，更优选15微米-900微米(0.15mm-0.9mm)，包括其间的所有值和范围，尤其是50、100、200、400、600和800微米。
抗冲改性聚酰胺的本发明膜可以用常规的方法挤出，例如在现有的膜生产线上挤出，并且可以根据需要提供非常薄的膜(例如5-50微米)。如上所述，膜可以是单层或多层。通过改变组成膜的材料的比例以及通过改变成膜工艺可以改变膜的性能。可以生产具有不同L1或L1/L2结构的两层膜而不需要粘结层。也可以制备三层或更多层的膜。由下列膜已经显著地获得了优异的效果：
-包含至少一层L1作为底层的膜；
-包含一层L1层作为底层的膜(单层膜)；
-包含至少两层L1层作为底层的膜；
-包含至少一层L1和至少一层L2作为底层的膜；
-包含两层作为底层的膜，第一层是L1层，另一层是L2层(双层膜)；在所述膜中，L1可以是内层或外层；
-包含L1/L2/L1三层作为底层的膜，其中L1既是内层又是外层，L2是中间层。
本发明的膜具有高拉伸性能和高抗冲强度，并表现出良好的耐磨性。通过双轴取向来提高机械强度、硬度和抗撕强度。因此，本发明的膜可用于经常使用聚酰胺膜的各种场合中但是提供更好的性能。
与传统的聚酰胺膜(PA 6或PA 66)相比，本发明的膜吸收水分更慢并且具有更低的透过率。因此，在一个实施方案中，本发明的膜可用于需要低渗透和较高温度的热水应用中。
与传统聚酰胺膜例如聚酰胺12、11、6或66膜相比，本发明的膜还对燃料和气体具有明显更低的渗透率。因此，在另一个实施方案中，本发明的膜可用于更高的温度并且可用于高温燃料系统应用中，特别是比传统聚酰胺膜更高的温度下。
在另一个实施方案中，本发明的膜可以在电动机和其它电子器件中用作绝缘器件。相对于传统聚酰胺膜例如PA12、PA11、PA66或PA6，本发明的膜在高湿度下具有更高的热性能和稳定的电性能，因此增进了本发明的膜在电子应用中的用途。
在另一个实施方案中，本发明的膜可用作柔性印刷电路和带式自动粘合层压体的基材。层压体可以粘合在膜的两面上并使用已知的丙烯酸树脂或环氧树脂来完成粘合。
本发明的膜还可在工业变压器中用于绝缘体以及压缩机发动机线圈绝缘体等。
本发明的膜对许多种物质具有优异的化学抵抗性，所述物质例如酯、酮、弱酸、脂族和芳族烃等。与传统的脂族聚酰胺例如PA6或66不同，本发明的膜对醇具有良好的抵抗性，因此，在另一个实施方案中，本发明的膜在制造或制备化学品时可用作耐腐蚀隔层。
实施例
下面提供本发明的示例性实施例，而不是限制性的。
表1描述了两种组合物。另外，对照组合物C1由未改性
A-1006PPA制备。
表1
利用挤出法来生产实施例1、2和C1的膜。对于这些实施例，利用共挤出/封铸来生产膜。图1A和图1B中示出了该方法所用设备。利用两台300mm挤出机E1和E2。使用标准聚乙烯和聚酰胺螺杆。挤出机经过进料挡板(feed block)与T型口模(T-die)连接。
PPA小球在挤出机E1中，高粘度管级别的聚乙烯(
B4922)在E2中。将PPA膜封铸在聚乙烯之间。PPA膜与聚乙烯膜没有粘合。很容易从HDPE层剥离中心PPA层。设备条件在表2中示出。
表2
| 实施例1 | 实施例2 | C1 | |
| 挤出机E1 | |||
| Z1 | 280 | 280 | 280 |
| Z2 | 315 | 300 | 315 |
| Z3 | 325 | 330 | 325 |
| Z4 | 325 | 300 | 325 |
| 挤出机E2 | |||
| Z1 | 150 | 280 | 150 |
| Z2 | 295 | 300 | 295 |
| Z3 | 325 | 330 | 325 |
| Z4 | 325 | 330 | 325 |
| 进料挡板 | 325 | 330 | 325 |
| 口模 | 325 | 330 | 325 |
根据螺杆转速和口模间隔不同，可以获得厚度为50-300微米的实施例1和2以及对照组C1的膜。
由这些膜来冲压ISO 1BA拉伸样品。以0.5mm/min的加载速度(crossheadspeed)对它们进行拉伸并在ISO 527条件下测试。如下表3所示，抗冲改性提供了具有比未改性对照组C1在屈服和断裂处更高的平均拉伸伸长率的聚合物组合物。实际上，包含抗冲改性剂的本发明PPA组合物具有超出对照组两倍的拉伸屈服和断裂伸长率。更高的拉伸屈服和断裂伸长率为本发明阻隔应用和热成型应用的工艺参数提供了更大的范围。
表3
膜挤出但不封铸
在18mm Brabender单螺杆机上实施配方实施例2。除用100mm宽的狭长口模替代T型口模外，设备与图1A中一样。
使用标准聚酰胺螺杆。机筒(barrel)设置从后到前为250至300℃。利用25mm的螺杆RPM和4kN的转矩，根据辊速不同获得50-150微米厚的膜。
大规模膜挤出
在工业规格(76mm直径)单螺杆设备上实施配方实施例2。螺杆为20∶1/L/D，并具有3∶1的压缩比。将辊加热到125℃。机筒(barrel)设置从后到前为310至325℃。接头和口模设置在330℃。利用70rpm的螺杆速度，根据机头压力不同以2-7米/分钟的速率生产0.4mm厚的膜。
利用ASTM D638测量上述膜的拉伸性能：
屈服拉伸强度＝54.6MPa
屈服伸长率＝5.2％
断裂拉伸强度＝67.8MPa
断裂伸长率＝110％
这清楚地表明制造抗冲改性剂聚邻苯二酰胺膜的商业实用性并且性能对于目标应用来说是可接受的。
阻隔性能
对实施例组合物、对照组和比较组合物进行燃料渗透试验。燃料渗透试验结果在下表4中示出。对来自如表3中所列的相同样品的膜实施燃料渗透试验。
除了抗冲改性组合物实施例1和2外，对PA 12、PA 6、
1010 PVDF和C1(Amodel A-1006)也实施渗透性测试。
测试的燃料是CTF1，体积比为45/45/10的异辛烷/甲苯/乙醇共混物。参见标准SAE J1681 rev.Jan.2000。
所测燃料渗透性以在1天时间内渗透通过厚度为1mm、表面积为1m2的板材的渗透克数表示。抗冲改性PPA、实施例1和2的渗透性远优于脂族聚酰胺(PA 6和PA12)并且与PVDF相似。
尽管本发明PPA组合物中引入弹性体通常被认为是对PPA的阻隔性能有害的，但是仍保持了非常好的阻隔性能。
表4
热成型
成功地热成型了0.4mm厚的实施例2的膜。将正方形的膜片夹在框架上，类似于油画布。将该框架引入到290-300℃的炉中持续15-45秒。将框架从炉中直接引到所述工装上。一旦进入适当位置，就启动所述工装，将膜热成型为所需制品。低于280℃的温度导致膜太硬从而不能成型。高于305℃的温度导致膜起泡或熔融。
冲压
利用工业设备成功地将0.4mm厚的实施例2的膜冲压成各种形状。这种技术对于形成电子工业用柔性电路板是有用的。
与PA12的热老化比较
表5描述了两种热稳定组合物(实施例3和实施例4)。
表5
表6提供了根据实施例3和4的组合物与热稳定PA12的比较。
表6
可以看出，热老化后PA12在悬臂梁式冲击强度方面损失巨大。因此，为了在空气存在下长期暴露于高温之后保持抗冲性能，部分芳族抗冲改性聚酰胺是更加安全的选择。
如本文所述，在本发明的某些实施方案中，膜包含L1组合物的单层结构。当用于本文中时，“单层”由一层聚合物组合物构成，其中聚合物组合物在层的整个厚度上是基本相同的。在本发明的某些实施方案中，单层的厚度可以是约0.05mm-约1.0mm。在本发明的某些实施方案中，单层的厚度是约0.15mm-约0.9mm。
膜可以具有粗糙、平滑、波纹状等的表面，整体具有恒定厚度或可变厚度等。另外，本发明膜可以用于封闭或封铸内含物，这些内含物可以大不一样。例如，本发明膜可用作保护系统。在这点上，实际上还以含有或装有其预定内含物的形式公开了本发明。
本发明的上述书面说明提供制造和使用它的方式和方法，使得本领域任何技术人员均能够制造并使用它，这种允许(enablement)具体提供为构成原始说明书一部分的所附权利要求的主题，并且包括膜，所述膜包含作为底层的
(1)包含芳族聚酰胺和抗冲改性剂的至少一层L1，和，任选的
(2)包含脂族聚酰胺的至少一层L2。
本发明的类似允许优选实施方案包括膜，其中芳族聚酰胺是聚邻苯二酰胺；脂族聚酰胺是脂族尼龙；抗冲改性剂选自EPDM、SEBS及其混合物；芳族聚酰胺是具有至少50mol％通过至少一种选自苯二甲酸、对苯二酸和间苯二酸及其混合物的二羧酸与至少一种脂族二胺之间的缩聚反应来获得的重复单元的聚酰胺；聚邻苯二酰胺包含约50mol％-约95mol％六亚甲基对苯二酰胺单元、约25mol％-约0mol％六亚甲基间苯二酰胺单元和约50mol％-约5mol％己二酰己二胺单元；抗冲改性剂是橡胶；橡胶是官能化聚烯烃基橡胶；官能化聚烯烃基橡胶是马来酸酐官能化苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物；官能化聚烯烃基橡胶是马来酸酐官能化乙烯-丙烯-二烯单体橡胶；层是次序为〔(L1)n/(L2)m〕x的邻接层，其中x是等于或大于1的任意整数，n是等于或大于1的任意整数，m是任意整数；层L1还包含外部润滑剂；外部润滑剂选自聚四氟乙烯、低密度聚乙烯及其混合物；层L1还包含含有至少一种铜(I)盐和至少一种碱金属卤化物的热稳定剂；热稳定剂包含至少一种选自碘化铜和溴化铜的卤化铜以及至少一种选自锂、钠和钾的碘化物和溴化物的碱金属卤化物；膜由作为底层的包含芳族聚酰胺和抗冲改性剂的单层组成；制造膜的方法，该膜包含作为底层的
(1)包含芳族聚酰胺和抗冲改性剂的至少一层L1，和，任选的
(2)包含脂族聚酰胺的至少一层L2，
该方法包括挤出芳族聚酰胺和抗冲改性剂以及任选地挤出脂族聚酰胺。
用于本文时，当某种聚合物被注明是“得自”或“包含”一个或多个单体(或单体单元)等时，这种说明是针对最终聚合物材料本身和其中全部或部分地构成该最终产物的重复单元。本领域普通技术人员理解，严格地说，聚合物不包括单个未反应的“单体”，而是由源自己反应单体的重复单元构成。
本文中提及的全部参考、专利、申请、试验、标准、文献、出版物、手册、文本、文章等通过引用并入本文。同样，所有可购买材料的所有手册、技术信息单等通过引用并入本文。在陈述数字限值或范围时，包括端值。此外，如果明确写出，则具体包括数字限值或范围内的所有值和子范围。
提供上述说明使得本领域技术人员能够制造和利用本发明，并且在具体应用及其要求的背景下提供上述说明。对优选实施方案的各种修改对本领域技术人员是显而易见的，本文限定的一般原理可适用于其它实施方案和应用而不偏离本发明的精神和范围。因此，本发明并不限于所示的实施方案，而是符合与本文公开的原理和特征一致的最大范围。
Claims (28)
1.膜，包含作为底层的
(1)包含芳族聚酰胺和抗冲改性剂的至少一层L1，和，任选的
(2)包含脂族聚酰胺的至少一层L2。
2.根据权利要求1所述的膜，其中所述芳族聚酰胺是聚苯二酰胺。
3.根据权利要求2所述的膜，其中所述膜包含至少一层L2，并且其中所述脂族聚酰胺是脂族尼龙。
4.根据权利要求1所述的膜，其中所述抗冲改性剂选自EPDM、SEBS及其混合物。
5.根据权利要求1所述的膜，其中所述芳族聚酰胺是具有至少50mol％通过至少一种选自邻苯二酸、对苯二酸和间苯二酸的二羧酸与至少一种脂族二胺之间的缩聚反应来获得的重复单元的聚酰胺。
6.根据权利要求2所述的膜，其中所述聚苯二酰胺包含50mol％-95mol％六亚甲基对苯二酰胺单元、25mol％-0mol％六亚甲基间苯二酰胺单元和50mol％-5mol％己二酰己二胺单元。
7.根据权利要求1所述的膜，其中所述抗冲改性剂是橡胶。
8.根据权利要求7所述的膜，其中所述橡胶是官能化聚烯烃基橡胶。
9.根据权利要求8所述的膜，其中所述官能化聚烯烃基橡胶是马来酸酐官能化苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物。
10.根据权利要求8所述的膜，其中所述官能化聚烯烃基橡胶是马来酸酐官能化乙烯-丙烯-二烯单体橡胶。
11.根据权利要求6所述的膜，其中所述抗冲改性剂选自马来酸酐官能化乙烯-丙烯-二烯单体橡胶、马来酸酐官能化苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物及其混合物。
12.根据权利要求1所述的膜，其中所述层是次序为〔(L1)n/(L2)m〕x的邻接层，其中x是等于或大于1的任意整数，n是等于或大于1的任意整数，m是任意整数。
13.根据权利要求1所述的膜，其中所述层L1还包含外部润滑剂。
14.根据权利要求13所述的膜，其中所述外部润滑剂选自聚四氟乙烯、低密度聚乙烯及其混合物。
15.根据权利要求1所述的膜，其中所述层L1还包含热稳定剂，所述热稳定剂包含至少一种铜(I)盐和至少一种碱金属卤化物。
16.根据权利要求15所述的膜，其中所述热稳定剂包含至少一种选自碘化铜和溴化铜的卤化铜以及至少一种选自锂、钠和钾的碘化物和溴化物的碱金属卤化物。
17.根据权利要求1所述的膜，由作为底层的包含芳族聚酰胺和抗冲改性剂的单层构成。
18.根据权利要求1所述的膜，其中层L1还包含抗氧化剂。
19.根据权利要求20所述的膜，其中所述抗氧化剂选自受阻酚、胺及其混合物。
20.制造膜的方法，所述膜包含作为底层的
(1)包含芳族聚酰胺和抗冲改性剂的至少一层L1，和，任选的
(2)包含脂族聚酰胺的至少一层L2，
所述方法包括挤出芳族聚酰胺和抗冲改性剂以及任选地挤出脂族聚酰胺以形成膜。
21.根据权利要求1所述的膜，包含作为底层的至少一层L1。
22.根据权利要求21所述的膜，包含作为底层的一层L1层。
23.根据权利要求21所述的膜，包含作为底层的至少两层L1层。
24.根据权利要求1所述的膜，包含作为底层的至少一层L1和至少一层L2。
25.根据权利要求24所述的膜，包含作为底层的两层，第一层是L1层，另外一层是L2层。
26.根据权利要求25所述的膜，其中L1是内层。
27.根据权利要求25所述的膜，其中L1是外层。
28.根据权利要求24所述的膜，其包含作为底层的三层L1/L2/L1，其中L1既是内层也是外层，L2是中间层。
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| CN2004800238813A Active CN1860003B (zh) | 2003-08-19 | 2004-08-17 | 抗冲改性聚酰胺中空体及其制作方法以及矿物燃料驱动装置 |
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2004
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- 2004-08-17 JP JP2006523972A patent/JP5048331B2/ja active Active
- 2004-08-17 EP EP04781335.7A patent/EP1658165B1/en active Active
- 2004-08-17 WO PCT/US2004/024383 patent/WO2005018891A1/en active Application Filing
- 2004-08-17 CA CA2535348A patent/CA2535348C/en not_active Expired - Fee Related
- 2004-08-17 EP EP20100182066 patent/EP2277675B1/en not_active Revoked
- 2004-08-17 BR BRPI0413653-5A patent/BRPI0413653A/pt not_active Application Discontinuation
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