CN105985634A - 包含evoh层的多层复合件 - Google Patents
包含evoh层的多层复合件 Download PDFInfo
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- CN105985634A CN105985634A CN201610149080.6A CN201610149080A CN105985634A CN 105985634 A CN105985634 A CN 105985634A CN 201610149080 A CN201610149080 A CN 201610149080A CN 105985634 A CN105985634 A CN 105985634A
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Abstract
本发明涉及包含EVOH层的多层复合件。其包含下列层并具有高的热变形温度、极好的抗冲强度、高的断裂伸长率和良好的层粘附:I.由包含至少40重量%的下列组分的模塑料制成的第一层(层I):1)60至99重量份的基于六亚甲基二胺、对苯二甲酸和具有8至19个碳原子的脂族二羧酸的共聚酰胺以及。2)40至1重量份的烯烃共聚物作为抗冲改性剂,其中1)和2)的重量份合计为100;和II.由模塑料制成的第二层(层II),所述模塑料的至少60重量%由EVOH构成;III.由聚酰胺模塑料制成的第三层。
Description
技术领域
本发明涉及多层复合件,其包含EVOH阻隔层和由基于抗冲改性的部分芳族聚酰胺的模塑料制成的层。该多层复合件主要是中空制品,例如用于传送或储存液体或气体介质的中空型材或容器。
背景技术
用作例如在机动车中传送液体或气体介质的管道的多层复合件的发展受到汽车工业对改进的阻隔效应的要求(特别是对燃料管路而言,以减少燃料组分排放到环境中)以及对足够的耐燃料性的要求。这导致开发出多层管道系统,其中例如使用乙烯-乙烯醇共聚物(EVOH)作为阻隔层材料。除EVOH层外还包含基于脂族聚酰胺的附加层的这类多层复合件例如从US 7 175 896已知。
因为在汽车应用中在发动机室中倾向于较高温度,在很多情况下脂族聚酰胺的热变形温度对于这类应用而言是不再足够的。因此自一段时间以来追求的是,通过部分芳族聚酰胺替代脂族聚酰胺。例如在WO 2005/018891中描述了中空制品,其包含至少一个由抗冲改性的部分芳族聚酰胺制成的层;其还可包含脂族聚酰胺层,但不包含附加层。该文献教导了,抗冲改性的部分芳族聚酰胺相对于PA12而言具有针对燃料组分扩散的改善的阻隔作用。但对于许多应用,恰好也在较高温度下,该阻隔作用仍是不够的。
由EP 2 666 823 A1已知,燃料管路可包含由抗冲改性的部分芳族聚酰胺制成的层以及例如由EVOH制成的阻隔层。US 2010/0035116 A1还描述了管道,其包含聚邻苯二甲酰胺外层,EVOH中间层和含氟聚合物内层。对于聚邻苯二甲酰胺的类型未作陈述。
在WO 2011/084423中研究了以下问题,即EVOH层不粘附在PA11或PA12层上并因此还需要增粘剂层。建议的是在这类复合件中将EVOH层与基于共聚酰胺的层组合,该共聚酰胺由10至40摩尔%的衍生自芳族二羧酸和脂族二胺的单元以及60至90摩尔%的衍生自脂族单体的单元构成。在实施例中使用具有25摩尔%的6T单元的PA612/6T和具有30摩尔%的6T单元的PA612/6T。然而,1.2至2.3 N/mm的与共挤EVOH层的粘附对于大多数技术应用而言是不够的。此外,这些示例性共聚酰胺具有198℃ 或197℃的微晶熔点(Kristallitschmelzpunkt)Tm,如WO 2012/106309的表3所示。它们的热变形温度因此是不够的。对于这些共聚酰胺的机械性能,在WO 2011/084423中未作陈述。
对于汽车应用,在发动机室中希望的是聚酰胺-EVOH-复合件,其中该聚酰胺具有至少240℃的微晶熔点Tm以及足够的结晶度。这些标准由可市购的结晶的部分芳族聚酰胺满足。但由于其差的机械性能,尤其是其差的抗冲韧性和小的断裂伸长率,它们并不适合于这类应用。在EP 2857456 A1中介绍了对于由分别具有30重量%的不同抗冲改性剂的PA6T/6I/66或者PA10T/TMDT制成的模塑料的测量;断裂伸长率为3至6 %。US 2014/0299220 A1给出了其它启示;其对比例22展示了包含800微米厚的由抗冲改性的PA6T/6I/66制成的层和200微米厚的ETFE层的管道,其中该管道的断裂伸长率为13%。在对比例24中展示了相应的管道,其聚酰胺层由抗冲改性的PA9T构成,其二胺成分为1,9-壬二胺和2-甲基-1,8-辛二胺的50 : 50-异构体混合物;在此断裂伸长率为22 %。最后对比例27展示了相应的管道,其聚酰胺层由抗冲改性的另一种PA6T/6I/66构成;在此断裂伸长率为18 %。但是,在该管道中希望的是更高的断裂伸长率,在某些应用中大于100%。该问题在目前情况中还由于以下问题而加剧,即EVOH是相对脆的,并因此必须嵌入在具有高的抗冲韧性和延展性的两层之间,由此可获得具有良好机械性能的管道。
因此本发明的目的在于,提供由EVOH层和至少两个聚酰胺层制成的复合件,其具有高的热变形温度、高的抗冲强度和高的断裂伸长率并且还获得良好的层粘附。还应提供使用内层材料的可能性,其中仅洗出极少量的低聚物并因此不在向发动机供应燃料时发生堵塞。
通过包含下列层的多层复合件实现这一目的:
I. 由包含至少40重量%,优选至少50重量%,特别优选至少60重量%,尤其优选至少70重量%,非常特别优选至少80重量%的下列组分的模塑料制成的第一层(层I):
1) 60至99重量份,优选65至98重量份,特别优选68至97重量份,尤其优选70至96重量份的由衍生自α)和β)的单体单元构成的部分芳族共聚酰胺
α) 41至90摩尔%,优选42至85摩尔%,特别优选43至80摩尔%,尤其优选44至75摩尔%,非常特别优选45至70摩尔%的六亚甲基二胺和对苯二甲酸的组合
β) 59至10摩尔%,优选58至15摩尔%,特别优选57至20摩尔%,尤其优选56至25摩尔%,非常特别优选55至30摩尔%的六亚甲基二胺和具有8至19个碳原子的线性脂族二羧酸的组合,
其中摩尔%值基于α)和β)的总和计,且其中最多20%,优选最多15%,特别优选最多12%,尤其优选最多8%,非常特别优选最多5%或最多4%的六亚甲基二胺可以被等量的其它二胺替代和/或其中最多20%,优选最多15%,特别优选最多12%,尤其优选最多8%,非常特别优选最多5%或最多4%的对苯二甲酸可以被等量的其它芳族二羧酸和/或1,4-环己烷二甲酸替代和/或其中最多20%,优选最多15%,特别优选最多12%,尤其优选最多8%,非常特别优选最多5%或最多4%的由六亚甲基二胺和线性脂族二羧酸构成的重复单元可以被等量的衍生自具有6至12个碳原子的内酰胺和/或ω-氨基羧酸的单元替代,
2) 40至1重量份,优选35至2重量份,特别优选32至3重量份,尤其优选30至4重量份的烯烃共聚物作为抗冲改性剂,
其中1)和2)的重量份合计为100;
II. 由模塑料制成的第二层(层II),所述模塑料的至少60重量%,优选至少70重量%,特别优选至少80重量%,尤其是优选至少90重量%和非常特别优选至少95重量%由EVOH构成;
III. 由聚酰胺模塑料制成的第三层。
层II优选地设置在层I和层III之间。
可考虑用作具有8至19个碳原子的线性脂族二羧酸的是:辛二酸(软木酸;C8)、壬二酸(杜鹃花酸;C9)、癸二酸(皮脂酸;C10)、十一烷二酸(C11)、十二烷二酸(C12)、十三烷二酸(C13)、十四烷二酸(C14)、十五烷二酸(C15)、十六烷二酸(C16)、十七烷二酸(C17)、十八烷二酸(C18)和十九烷二酸(C19)。
根据权利要求,六亚甲基二胺的一部分可任选被其它二胺替代。原则上,各种二胺在此都合适;例举下列二胺:1,10-癸二胺、1,12-十二烷二胺、间苯二甲胺、对苯二甲胺、双(4-氨基环己基)甲烷、2-甲基-1,5-戊二胺和1,4-双-氨基甲基环己烷。当然也可以使用此类二胺的混合物。但是,优选除六亚甲基二胺外不使用其它二胺。
根据权利要求,对苯二甲酸的一部分也可任选被其它芳族二羧酸或被1,4-环己烷二甲酸替代。原则上,各种芳族二羧酸在此都合适;例举下列二羧酸:间苯二甲酸、4,4'-二苯基二甲酸、4,4'-二苯基醚二甲酸、2,6-萘二甲酸、1,4-萘二甲酸和1,5-萘二甲酸。当然也可以使用此类二羧酸的混合物。但是,优选除对苯二甲酸外不使用其它芳族二羧酸和/或不使用1,4-环己烷二甲酸。类似地,根据权利要求,由六亚甲基二胺和线性脂族二羧酸构成的重复单元的一部分可任选被具有6至12个碳原子的内酰胺和/或ω-氨基羧酸替代。在此,由六亚甲基二胺和线性脂族二羧酸构成的重复单元对应于源自内酰胺和/或ω-氨基羧酸的单元。具有6至12个碳原子的内酰胺和/或ω-氨基羧酸的实例包括己内酰胺、辛内酰胺、十一内酰胺、ω-氨基十一烷酸、月桂内酰胺和ω-氨基十二烷酸。在此优选的是具有11或12个碳原子的内酰胺和/或ω-氨基羧酸。但是,优选除六亚甲基二胺和线性脂族二羧酸外不使用内酰胺和/或ω-氨基羧酸。
有利地选择该部分芳族共聚酰胺的组成,以使其根据ISO 11357在第二次加热时测得的微晶熔点Tm为240℃至300℃,优选250℃至295℃,特别优选260℃至290℃。当出现多个熔融峰时,由主熔融峰确定Tm。
该共聚酰胺通常通过熔融缩聚制备。相应的方法是现有技术。也可以使用各种其它已知的聚酰胺合成方法。
在确保这些单体可以以1:1摩尔比反应时,则存在六亚甲基二胺和对苯二甲酸的必要等摩尔组合。在此可以考虑,六亚甲基二胺相对易挥发,因此在缩聚过程中可能发生损失,这需要用较大的装料量(Einwaage)补偿。还可能必须略微偏离确切的化学计量,以建立特定的端基比。这同样适用于1)ß) 六亚甲基二胺和具有8至19个碳原子的线性脂族二羧酸的必要等摩尔组合。
在一个优选实施方案中,该部分芳族聚酰胺的氨基端基与氨基和羧基端基总和的比率为0.3至0.7,特别优选0.35至0.65。可以通过使用本领域技术人员已知的方法调节缩聚,设定氨基端基的含量。可以例如通过改变所用二胺与所用二羧酸的比率、通过添加单羧酸或通过添加单胺实现所述调节。也可以通过以粒料或熔体形式混合两种共聚酰胺(其中一种富含氨基端基,另一种具有少的氨基端基)来设定氨基端基的含量。
可以通过使用高氯酸滴定该共聚酰胺的间甲酚溶液来测定氨基含量。可以通过用KOH/乙醇滴定该共聚酰胺的邻甲酚溶液来实现羧基含量的测定。这些方法是本领域技术人员熟悉的。
该抗冲改性剂特别是包含下列单体的单元的烯烃共聚物:
a) 20至99.9重量%,优选30至99.7重量%的一种或多种具有2至12个碳原子的α-烯烃,
b) 0至50重量%的一种或多种丙烯酸类化合物,其选自
- 丙烯酸、甲基丙烯酸或其盐和
- 丙烯酸或甲基丙烯酸与C1至C12醇的酯,其中排除含环氧基的酯,如丙烯酸缩水甘油酯和甲基丙烯酸缩水甘油酯,
c) 0.1至50重量%的烯类不饱和环氧化物或二羧酸酐,
其中重量%值基于该烯烃共聚物计,合计可为最大100。应考虑到,可另外存在衍生自其它共聚单体,例如衍生自苯乙烯或非共轭二烯的单元。
当组分c)由衍生自不饱和二羧酸酐的单元构成时,它们优选以0.1至8重量%,特别优选0.3至5重量%的量存在。
当组分c)由衍生自烯类不饱和环氧化物的单元构成时,根据b)的丙烯酸类化合物既不含丙烯酸也不含甲基丙烯酸。
在第一实施方案中,该抗冲改性剂是包含下列单体单元的烯烃共聚物:
- 35至94.9重量%,优选40至90重量%,特别优选45至85重量%的基于乙烯的单体单元,
- 5至65重量%,优选10至60重量%,特别优选15至55重量%的基于具有4至8个碳原子的1-烯烃的单体单元,
- 0至10重量%的基于其它烯烃的单体单元和
- 0.1至2.5重量%的基于脂族不饱和二羧酸酐的单体单元,
其中选择各个含量,以使这些重量%值合计为100。基于乙烷的单体单元根据本发明的进一步下限为34.9重量%,优选39.9重量%,特别优选44.9重量%,而其根据本发明的进一步上限优选为89.9重量%,特别优选84.9重量%。
可考虑作为具有4至8个碳原子的1-烯烃用于该烯烃共聚物的是下列化合物:1-丁烯、1-戊烯、1-己烯、1-庚烯和1-辛烯。当然,基于具有4至8个碳原子的1-烯烃的单体单元也可源自这些化合物的混合物。
对其单体单元构成该烯烃共聚物的0至10重量%的其它烯烃的类型没有限制。例如,所述烯烃可以是非共轭二烯、单烯如丙烯、4-甲基-1-戊烯或苯乙烯或其混合物。
在第一变型中,其单体单元构成该烯烃共聚物的0至10重量%的其它烯烃不是非共轭二烯。
在第二变型中,这种其它烯烃不是苯乙烯和/或不是丙烯。
在第三变型中,该烯烃共聚物仅含衍生自乙烯、具有4至8个碳原子的1-烯烃和脂族不饱和二羧酸酐的单体单元。
在第四变型中,具有4至8个碳原子的1-烯烃是1-丁烯。
在第五变型中,具有4至8个碳原子的1-烯烃是1-己烯。
在第六变型中,具有4至8个碳原子的1-烯烃是1-辛烯。
这些变型可以不受限制地互相组合。
该脂族不饱和二羧酸酐可以是例如马来酸酐,但其它相应的化合物如乌头酸酐、柠康酸酐或衣康酸酐也合适。
根据权利要求的烯烃共聚物可以以已知方式制备,其中通过热或优选通过自由基方式使脂族不饱和二羧酸酐或其前体例如相应的酸或半酯与预制的共聚物反应。在此该脂族不饱和二羧酸酐也可以与其它单体,例如与富马酸二丁酯或苯乙烯组合着反应。根据权利要求的烯烃共聚物可以以各种类型商业购得。
在第二实施方案中,该抗冲改性剂是包含下列单体单元的烯烃共聚物:
- 35至94.9重量%,优选40至90重量%,特别优选45至85重量%的基于乙烯的单体单元,
- 5至65重量%,优选10至60重量%,特别优选15至55重量%的基于丙烯的单体单元,
- 0至10重量%的基于其它烯烃例如非共轭二烯的单体单元,和
- 0.1至2.5重量%的基于脂族不饱和二羧酸酐的单体单元,
其中选择各个含量,以使这些重量%值合计为100。基于乙烷的单体单元根据本发明的进一步下限为34.9重量%,优选39.9重量%,特别优选44.9重量%,而其根据本发明的进一步上限优选为89.9重量%,特别优选84.9重量%。
在第三实施方案中,该抗冲改性剂是包含至少一个聚乙烯基芳族嵌段A和至少一个聚烯烃嵌段B的氢化和酸酐改性的嵌段共聚物。这些嵌段可以以线性或星形方式排列,例如以A-B、A-B-A、B-A-B、A-B-A-B、A-B-A-B-A、B-A-B-A-B、(A)B3、(B)A3、(A)(B-A)3、(B)(A-B)3类型的结构,其中这些嵌段共聚物的数均分子量为大约10000至大约800000,优选大约20000至大约500000。该嵌段共聚物中乙烯基芳族化合物的含量优选为10至70重量%,特别优选10至55重量%。类似橡胶的聚烯烃嵌段B包含例如乙烯/丙烯、乙烯/丁烯或乙烯/戊烯单元;它们通过共轭二烯,特别是丁二烯、异戊二烯、1,3-戊二烯、2,3-二甲基丁二烯或其混合物的聚合和随后选择性的氢化获得。在这种情况下,将聚合的二烯的部分中的脂族双键的至少80%,优选至少90%,特别优选至少94%氢化。用于制备该聚乙烯基芳族嵌段的乙烯基芳族化合物通常是苯乙烯,但也可以例如使用α-甲基苯乙烯等。氢化的嵌段共聚物包含0.1至8重量%,优选0.3至5重量%的琥珀酸酐基团,其通过在氢化前或优选在氢化后与不饱和二羧酸或其酸酐如马来酸酐、柠康酸、衣康酸等反应来引入。这样的酸酐改性的氢化的乙烯基芳族化合物/共轭二烯嵌段共聚物的制备是现有技术;合适的类型可商业购得,例如以商品名Kraton® FG1901X。这是具有30重量%的聚苯乙烯含量和1.4至2重量%的琥珀酸酐基团含量的SEBS型(苯乙烯-乙烯/丁烯-苯乙烯)线性三嵌段共聚物。
在第四实施方案中,该抗冲改性剂是下列组分的混合物
- 5至95重量%的包含下列单体的单元的烯烃共聚物:
a) 20至99.9重量%的一种或多种具有2至12个碳原子的α-烯烃,
b) 0至50重量%的丙烯酸或甲基丙烯酸与C1至C12醇的酯,其中排除含环氧基的酯,和
c) 0.1至50重量%的烯类不饱和环氧化物,
其中重量%值基于该烯烃共聚物计,并合计为最大100,和
- 95至5重量%的包含下列单体的单元的烯烃共聚物:
a) 42至99.9重量%的一种或多种具有2至12个碳原子的α-烯烃,
b) 0至50重量%的丙烯酸或甲基丙烯酸与C1至C12醇的酯,其中排除含环氧基的酯,和
c) 0.1至8重量%的烯类不饱和二羧酸酐,
其中重量%值基于该烯烃共聚物计,并合计为最大100。
具有2至12个碳原子的α-烯烃例如选自乙烯、丙烯、1-丁烯、1-戊烯、4-甲基戊-1-烯、1-己烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯、1-十一碳烯和1-十二碳烯,优选的是乙烯。
丙烯酸或甲基丙烯酸的酯的实例特别包括丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸2-乙基己酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丁酯和甲基丙烯酸2-乙基己酯。
烯类不饱和环氧化物的实例特别包括缩水甘油酯和缩水甘油醚,如丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、马来酸缩水甘油酯、衣康酸缩水甘油酯、乙烯基缩水甘油醚和烯丙基缩水甘油醚。
烯类不饱和二羧酸酐的实例包括马来酸酐、衣康酸酐、柠康酸酐、2,3-二甲基马来酸酐和(2.2.2)双环辛-5-烯-2,3-二甲酸酐。
在第五实施方案中,该抗冲改性剂是下列组分的混合物
- 70至99重量%的来自第一实施方案的抗冲改性剂和
- 1至30重量%的包含下列单体的单元的烯烃共聚物:
a) 20至99.9重量%的一种或多种具有2至12个碳原子的α-烯烃,
b) 0至50重量%的丙烯酸或甲基丙烯酸与C1至C12醇的酯,其中排除含环氧基的酯,和
c) 0.1至50重量%的烯类不饱和环氧化物,
其中重量%值基于该烯烃共聚物计,并合计最大100。
此处所用的烯烃共聚物的细节与对第四实施方案描述的相同。
在第六实施方案中,该抗冲改性剂是下列组分的混合物
- 70至99重量%的来自第二实施方案的抗冲改性剂和
- 1至30重量%的包含下列单体的单元的烯烃共聚物:
a) 20至99.9重量%的一种或多种具有2至12个碳原子的α-烯烃,
b) 0至50重量%的丙烯酸或甲基丙烯酸与C1至C12醇的酯,其中排除含环氧基的酯,和
c) 0.1至50重量%的烯类不饱和环氧化物,
其中重量%值基于该烯烃共聚物计,并合计最大100。
此处所用的共聚物的细节与对第四实施方案描述的相同。
在第七实施方案中,该抗冲改性剂是下列组分的混合物
- 50至99重量%的来自第一实施方案的抗冲改性剂和
- 1至50重量%的来自第三实施方案的氢化和酸酐改性的嵌段共聚物。
在第八实施方案中,该抗冲改性剂是下列组分的混合物
- 50至99重量%的来自第二实施方案的抗冲改性剂和
- 1至50重量%的来自第三实施方案的氢化和酸酐改性的嵌段共聚物。
这些实施方案仅是示例性的。在本发明中也可以使用本文中没有提到的其它抗冲改性剂。第一实施方案在此特别优选,因为这样的模塑料具有特别高的热老化耐受性。同样包含来自第一实施方案的抗冲改性剂的第五和第七实施方案也优选。
除组分1)和2)外,根据本发明使用的层I的模塑料任选含有附加添加剂,它们将平衡补足至100重量%,并优选为其中的至少0.01重量%。这些附加添加剂的实例包括:
a) 稳定剂,
b) 其它聚合物,
c) 增塑剂,
d) 颜料和/或染料,
e) 提高导电性的添加剂和
f) 加工助剂。
在一个优选实施方案中,该模塑料含有有效量的含铜稳定剂。这特别是可溶于聚酰胺基质的铜化合物。该铜化合物优选与碱金属卤化物组合。
在某些实施方案中,该稳定剂是与碱金属卤化物组合的铜(I)盐,例如乙酸铜、硬脂酸铜、有机铜络合物例如乙酰丙酮铜、卤化铜等。
在某些实施方案中,该含铜稳定剂包含选自碘化铜和溴化铜的卤化铜和选自锂、钠和钾的碘化物和溴化物的碱金属卤化物。
优选进料加入含铜稳定剂,以使得模塑料含有20至2000 ppm铜,特别优选30至1500 ppm铜,尤其优选40至1000 ppm铜。
更优选含铜稳定剂的组成,以使得碱金属卤化物与铜化合物的重量比为2.5至12,特别优选6至10。碱金属卤化物和铜化合物的组合通常以大约0.01重量%至大约2.5重量%的量包含于模塑料中。
该含铜稳定剂对长期热老化提供防护,例如在汽车的发动机罩下的用途中。
在另一个优选实施方案中,该模塑料包含有效量的氧化稳定剂,特别优选与有效量的含铜稳定剂组合的有效量的氧化稳定剂。合适的氧化稳定剂的实例包括芳胺、位阻酚、亚磷酸酯、亚膦酸酯、含硫增效剂、羟胺、苯并呋喃酮衍生物、丙烯酰基改性的酚等。许多类型的这种氧化稳定剂可商业购得,例如以商品名Naugard 445、Irganox 1010、Irganox1098、Irgafos 168、P-EPQ或Lowinox DSTDP。该模塑料通常包含大约0.01至大约2重量%,优选大约0.1至大约1.5重量%的氧化稳定剂。
该模塑料还可包含UV稳定剂和/或HALS型光稳定剂。合适的UV稳定剂主要是有机UV吸收剂,例如二苯甲酮衍生物、苯并三唑衍生物、 草酰苯胺或苯基三嗪。HALS型光稳定剂是四甲基哌啶衍生物;这些是充当自由基捕获剂的抑制剂。UV稳定剂和光稳定剂可以有利地组合着使用。许多类型的这两者可商业购得;关于用量,可以遵循制造商的指示。
该模塑料可另外包含水解稳定剂,例如单体、低聚或聚合碳二亚胺或双噁唑啉。
可作为添加剂包含于该模塑料中的其它聚合物的实例包括脂族聚酰胺、聚醚酰胺或聚四氟乙烯(PTFE)。
合适的脂族聚酰胺的实例包括PA46、PA66、PA68、PA610、PA612、PA613、PA410、PA412、PA810、PA1010、PA1012、PA1013、PA1014、PA1018、PA1212、PA6、PA11和PA12以及衍生自这些类型的共聚酰胺。由所述部分芳族共聚酰胺、任选脂族聚酰胺和任选聚醚酰胺构成的模塑料的聚酰胺部分优选包含少于10重量%,特别优选少于8重量%,尤其优选少于5重量%,非常特别优选少于3重量%的脂族聚酰胺或优选少于10重量%,特别优选少于8重量%,尤其优选少于5重量%,非常特别优选少于3重量%的脂族聚酰胺和聚醚酰胺的总和。
增塑剂及其在聚酰胺中的应用是已知的。适用于聚酰胺的增塑剂的综述可见于Gächter/Müller, Kunststoffadditive [Plastics additives], C. Hanser Verlag, 第2版, 第296页。
适合用作增塑剂的常规化合物的实例包括在醇组分中具有2至20个碳原子的对羟基苯甲酸的酯或在胺组分中具有2至12个碳原子的芳基磺酸的酰胺,优选苯磺酸的酰胺。可考虑的增塑剂尤其包括对羟基苯甲酸乙酯、对羟基苯甲酸辛酯、对羟基苯甲酸异十六烷基酯、甲苯磺酸正辛基酰胺、苯磺酸正丁基酰胺或苯磺酸2-乙基己基酰胺。
合适的颜料和/或染料的实例包括炭黑、氧化铁、硫化锌、群青、苯胺黑、珠光颜料和金属片。
提高导电性的添加剂的实例包括导电炭黑或碳纳米管。
合适的加工助剂的实例包括链烷烃、脂肪醇、脂肪酸酰胺、硬脂酸酯/盐如硬脂酸钙、石蜡、褐煤酸酯/盐或聚硅氧烷。
由各成分以本领域技术人员已知的方式通过熔融形式混合制备该模塑料。
第二层的EVOH是由乙烯和乙烯醇构成的共聚物;其有时也称为EVAL。该共聚物中的乙烯含量通常为22至60摩尔%和特别是28至45摩尔%。可商业获得多种类型。例如可参阅来自Kuraray EVAL Europe的公司文件“Introduction to Kuraray EVALTM Resins”,第1.2/9810版。除根据现有技术的EVOH外,所述模塑料还可包含如对于阻隔层应用常见的附加添加剂。这类添加剂通常是EVOH-供应商的专有知识。
第三层的聚酰胺模塑料可与第一层的聚酰胺模塑料相同种类。此外可选地,该聚酰胺模塑料还可基于脂族聚酰胺构成。合适的脂族聚酰胺例如是PA46、PA66、PA68、PA610、PA612、PA613、PA410、PA412、PA810、PA1010、PA1012、PA1013、PA1014、PA1018、PA1212、PA6、PA11和PA12以及衍生自这些类型的共聚酰胺。在此优选微晶熔点Tm在190℃以上,特别优选在200℃以上,尤其优选在210℃以上的脂族聚酰胺。
基于脂族聚酰胺的聚酰胺模塑料包含至少40重量%,优选至少50重量%,特别优选至少60重量%和尤其优选至少70重量%的脂族聚酰胺;其还可包含抗冲改性剂以及常见的添加剂,例如对于第一层模塑料所述类型的那些。
本发明的多层复合件可以是平面复合件的形式,例如片材或薄膜的形式,例如利用EVOH对于气体例如氧气和二氧化碳的阻隔作用的包装膜的形式,或用于近海开采的柔性管的防磨带的形式。
在一个优选实施方案中,本发明的多层复合件是中空制品,主要是管道或容器。这包括例如燃料管路、液压管路、制动压缩空气管路、离合器管路或冷却液管路、制动液容器或燃料容器。其它用途是例如石油或天然气开采工业中的硬质或柔性管道的内衬(Liner)或传送热液体的脐带(Umbilical)管。当内层与汽油或生物柴油接触时,其优选不含铜稳定剂。
意想不到地发现,基于要求保护的部分芳族共聚酰胺的层良好地粘附在EVOH层上。在关于应用时要求还更牢固粘附的情况下,这可借助插入之间的增粘剂层来实现。合适的增粘剂例如是聚酰胺或聚酰胺共混物,其既可与第一层也可与第二层相容,例如基于PA6、PA66的模塑料、要求保护的抗冲改性的部分芳族聚酰胺与PA6和/或PA66或增粘剂的共混物,其如由US 7 175 896已知,例如PA6/PA612共混物,其可借助酸酐官能化的橡胶进行抗冲改性。
当本发明的多层复合件用于传送或储存可燃液体、气体或粉尘,例如燃料或燃料蒸气时,建议为属于该复合件的层之一或附加内层提供导电性。这可通过根据现有技术的所有方法与导电添加剂配混来实现。可用的导电添加剂的实例包括导电炭黑、金属片、金属粉、金属化的玻璃珠、金属化的玻璃纤维、金属纤维(例如来自不锈钢)、金属化的晶须、碳纤维(还有金属化的)、固有导电聚合物或石墨原纤。也可以使用各种导电添加剂的混合物。
该导电层在优选的情况下与要传送或储存的介质直接接触并具有最大109 Ω/方的比表面电阻。在2004年11月的SAE J 2260中阐明测定多层管的电阻的测量方法。
当本发明的多层复合件制作为中空制品或中空型材(例如管道)时,该多层复合件还可以用附加弹性体层包覆。交联橡胶物料和热塑性弹性体都适用于该包覆。该包覆套可以使用或不使用附加增粘剂施加到该多层复合件上,例如通过经十字模头挤出或通过将预制的弹性体软管推在预先挤出的多层管上。该包覆套通常具有0.1至4毫米,优选0.2至3毫米的厚度。
合适的弹性体的实例包括氯丁二烯橡胶、乙烯-丙烯橡胶(EPM)、乙烯-丙烯-二烯橡胶(EPDM)、表氯醇橡胶(ECO)、氯化聚乙烯、丙烯酸酯橡胶、氯磺化聚乙烯、硅酮橡胶、山都平(Santoprene)、聚醚酯酰胺或聚醚酰胺。
该多层复合件可以在单级或多级程序中制造,例如通过借助多组分注塑、共挤、共挤吹塑(还例如3D吹塑、型坯挤出(Schlauchextrusion)到开放半模中、3D型坯控制(Schlauchmanipulation)、吸吹成型、3D吸吹成型、连续吹塑)的单级法或通过如例如US 5554 425中描述的多级法。
下表列出可能的示例性层构造。这些实例仅用于举例说明而不应限制本发明的范围。所提到的层构造普遍适用,无论几何形状如何,即也适用于薄膜。但是,所述层构造也特别适用于中空制品,如中空型材,例如管道或容器;在这种情况下根据a)的层是外层。
本发明的复合件具有高的热变形温度、非常好的抗冲强度和高的断裂伸长率。在没有使用增粘剂的情况下,层粘附就已如此良好,以使其对于大多数应用而言是足够的。此外表明,当根据本发明使用的层 I的模塑料作为内层存在时,从其中仅洗出极少量的低聚物;因此不在向发动机供应燃料时发生堵塞。本发明的管道针对燃料组分的阻隔作用是极好的。
具体实施方式
下面示例性说明本发明。
在实施例中使用下列材料:
PA6T/612: 见制备实施例1
色母料(Farbbatch): 80重量% PA12和20重量%炭黑的混合物
TAFMER® MH7010: 来自Mitsui Chemicals的酸酐改性的乙烯-丁烯橡胶
硬脂酸钙: 加工助剂
Polyad® PB201碘化物: 基于碘化铜的含铜稳定剂和碱金属卤化物
Naugard® 445: 氧化稳定剂(芳胺)
增粘剂: 由62.13重量份的PA612、15.93重量份的PA6、7.97重量份的增塑剂(BBSA)、11.15重量份的抗冲改性剂和1.22重量份的稳定剂制成的模塑料
EVOH: EVAL® FP101B,来自KURARAY的具有32摩尔%乙烯的EVOH
PA12: VESTAMID® LX9002,抗冲改性的增塑的PA12挤出模塑料
HI-PA6T/612: 根据本发明使用的抗冲改性的PA6T/612模塑料。
制备实施例1 (PA6T/612 50:50):
首先向缩聚容器中装入12.621千克六亚甲基二胺、9.021千克对苯二甲酸、13.356千克十二烷二酸、15.000千克蒸馏水和3.53克50重量%次磷酸水溶液。将原材料在180℃下熔融并在225℃/22巴下搅拌3小时。在连续减压至10巴的情况下加热至300℃,然后在此温度下进一步减压。在达到0.5巴时,将该容器排空并将产物造粒。在转鼓式干燥机中将该粒料进行后缩合并由此达到所需分子量。
微晶熔点Tm: 278℃(主峰)。
根据本发明使用的模塑料(HI-PA6T/612)的制备:
使用65.38重量份所制备的PA6T/612、30重量份TAFMER MH7010、2.5重量份色母料、1.2重量份Polyad PB201碘化物、0.6重量份Naugard 445和0.32重量份硬脂酸钙。由各成分通过在捏合装置中熔融混合制备该模塑料,然后以条状形式输出、造粒和干燥。
参比例:
使用来自IDE的型号ME 45/4 x 25D的单层管(Monorohr)挤出装置由根据本发明使用的模塑料在280℃和100 转/分钟的转数下制造具有8.0毫米外径和1.0毫米壁厚的单层管。
实施例1至3:
在每种情况中使用来自Bellaform的多层管装置制造具有8.0毫米外径和1.0毫米总壁厚的多层管。层构造显示在表1中。
试验:
a) 拉伸试验: 根据DIN EN ISO 527-1以100 mm/min的拉拔速度测试单层和多层管。试样具有大约200毫米长度,夹紧长度为100毫米,且应变传感器间距为50毫米。
b) 冲击弯曲试验: 根据DIN 73378在23℃和-40℃下进行单层和多层管的抗冲韧性测量。对此分别使用10个长度大约100毫米的管段。
c) 落锤试验: 根据SAE规范进行落锤试验。在此使特定重物从规定落高落到试样上。通过这一试验根据SAE J2260和SAE J844测定单层和多层管在冲击作用下的抗冲韧性特性。分别在-40℃下测量10个试样,并在经受试验后目视检查损坏。
d) 分离试验: 用来自Zwick的BZ 2.5/TN1S拉力试验机(其上固定有拉伸装置和旋转金属轮以能够将试样的各层彼此分离)进行分离试验。经由根据DIN EN ISO 2411的分离试验通过测量将两层彼此分离所需的力来评估两层之间的粘附。为此,使用切割装置从该多层管上纵向分割出三份长度20厘米的管段。
在开始测量前,使用卡尺在不同位置处反复测量样品宽度并将平均值输入评估软件。然后将一层的初分离的末端夹入夹具中,该夹具将该层以90°的角度连续与第二层拉开。
以50 mm/min的试验速度拉开层,同时记录以牛顿为单位的所需力与以毫米为单位的路程的图。由此图确定以N/mm为单位的分离阻力,其与粘附接触面积的宽度相关联。
e) 燃料渗透性:通过渗透测量测定,在60℃下静态储存时每天和每米管道或每平方米管道内表面通过燃料管路渗透多少燃料。对此分别称量300毫米长的管段,随后用300毫升CE10(组成:45体积%的甲苯、45体积%的异辛烷和10体积%的乙醇)装填并密封两端。再次称量装填的管道,以能够在特定时间段内测定质量损失和由此测定渗透的燃料质量。有效的渗透长度在此为285毫米。
结果显示在表1中。
低聚物洗出稳定性:
通过低聚物洗出稳定性,测试由试验燃料从每米管道中洗出的可溶和不可溶提出物的质量。对于这一试验,将含醇试验燃料FAM B(42.3体积%甲苯、25.4体积%异辛烷、4.3体积%乙醇、12.7体积%二异丁烯、15.0体积%甲醇和0.5体积%去离子水)在2米长的管段中在60℃下储存72小时。各管道的一端用金属球密封以准备样品。用试验燃料将试样填充至大约95%并密封,然后在60℃下置于循环空气炉中。在经过72小时的试验时间后,取出管道,冷却至室温并短暂摇振以溶解管道内壁上的可能的残留物。将各试验液体分别填充到玻璃烧杯中,冷却至0℃并在此温度下储存另外24小时。使用具有0.045微米孔径的聚醚砜(PES)过滤器吸滤出试验液体中包含的不溶提出物,然后称重。然后将滤液在通风橱中蒸发24小时,并将残留物称重。分别进行三重测定。
从来自实施例1的管道获得每米管道1.2毫克的不溶提出物和在滤液蒸发后每米管道135毫克的残留物。
用于比较: 在相同程序后,从由PA12模塑料VESTAMID® X7293(其通常用作多层管中的内层)制成的单层管获得每米管道15.9毫克的不溶提出物和在滤液蒸发后每米管道853毫克的残留物。
本发明的管道因此符合对燃料管路所提出的要求。
Claims (14)
1.多层复合件,其包含下列层:
I. 由包含至少40重量%的下列组分的模塑料制成的第一层(层I):
1) 60至99重量份的部分芳族共聚酰胺,其由衍生自α)和β)的单体单元构成:
α) 41至90摩尔%的六亚甲基二胺和对苯二甲酸的组合
β) 59至10摩尔%的六亚甲基二胺和具有8至19个碳原子的线性脂族二羧酸的组合;
其中所述摩尔%值基于α)和β)的总和计,且其中最多20%的六亚甲基二胺可以被等量的其它二胺替代和/或其中最多20%的对苯二甲酸可以被等量的其它芳族二羧酸和/或1,4-环己烷二甲酸替代和/或其中最多20%的由六亚甲基二胺和线性脂族二羧酸构成的重复单元可以被等量的衍生自具有6至12个碳原子的内酰胺和/或ω-氨基羧酸的单元替代,
2) 40至1重量份的烯烃共聚物作为抗冲改性剂,
其中1)和2)的重量份合计为100;
II. 由模塑料制成的第二层(层II),所述模塑料的至少60重量%由EVOH构成;
III. 由聚酰胺模塑料制成的第三层。
2.根据权利要求1的多层复合件,其特征在于层I的模塑料包含0.01至60重量%的附加添加剂。
3.根据权利要求2的多层复合件,其特征在于所述附加添加剂之一是含铜稳定剂。
4.根据权利要求2和3任一项的多层复合件,其特征在于所述附加添加剂之一是氧化稳定剂。
5.根据前述权利要求任一项的多层复合件,其特征在于根据ISO 11357在第二次加热时测得的层I的共聚酰胺的微晶熔点Tm为240℃至300℃。
6.根据前述权利要求任一项的多层复合件,其特征在于,层 II的模塑料的EVOH包含22至60摩尔%的乙烯单元。
7.根据前述权利要求任一项的多层复合件,其特征在于,所述第三层的聚酰胺模塑料与第一层的聚酰胺模塑料是相同种类的。
8.根据权利要求1至6任一项的多层复合件,其特征在于,所述第三层的聚酰胺模塑料基于脂族聚酰胺构成。
9.根据前述权利要求任一项的多层复合件,其特征在于,所述多层复合件包含一个或多个附加层。
10.根据前述权利要求任一项的多层复合件,其特征在于所述多层复合件是薄膜、片材或中空制品。
11.根据权利要求10的多层复合件,其特征在于,所述中空制品为中空型材,特别是管道或容器。
12.根据权利要求11的多层复合件,其特征在于,所述多层复合件包含一个或多个选自导电层和弹性体包覆套的附加层。
13.根据权利要求11和12任一项的多层复合件,其特征在于,所述多层复合件是燃料管路、液压管路、制动压缩空气管路、离合器管路、冷却液管路、石油或天然气开采工业中的硬质或柔性管道的内衬或脐带管。
14.根据权利要求11和12任一项的多层复合件,其特征在于,所述多层复合件是制动液容器或燃料容器。
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CN113544213A (zh) * | 2019-03-06 | 2021-10-22 | 巴斯夫欧洲公司 | 用于高光泽应用的聚酰胺模塑组合物 |
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EP3222668B1 (en) * | 2014-11-20 | 2023-07-19 | Toray Industries, Inc. | Use of a hose and use of a polyamide composition for preparing an inner layer of the hose coming into contact with high-pressure hydrogen |
FR3046826B1 (fr) | 2016-01-15 | 2018-05-25 | Arkema France | Structure tubulaire multicouche possedant une meilleure resistance a l'extraction dans la bio-essence et son utilisation |
MX2020002840A (es) | 2017-09-28 | 2020-10-12 | Dupont Polymers Inc | Proceso de polimerizacion. |
WO2019065231A1 (ja) | 2017-09-29 | 2019-04-04 | 宇部興産株式会社 | 積層チューブ |
EP3477176A1 (de) | 2017-10-25 | 2019-05-01 | Evonik Degussa GmbH | Verfahren zur herstellung eines mit einem inliner ausgekleideten rohres |
DE102018213140A1 (de) * | 2018-08-06 | 2020-02-06 | Aft Automotive Gmbh | Mehrschichtverbund sowie Fluidleitung |
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CN111511551A (zh) * | 2017-12-22 | 2020-08-07 | Ems 专利股份公司 | 柔性塑料管路以及用于其制造的方法和其应用 |
CN113544213A (zh) * | 2019-03-06 | 2021-10-22 | 巴斯夫欧洲公司 | 用于高光泽应用的聚酰胺模塑组合物 |
Also Published As
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US10252498B2 (en) | 2019-04-09 |
JP6887218B2 (ja) | 2021-06-16 |
MX2016003330A (es) | 2016-09-16 |
EP3069871A1 (de) | 2016-09-21 |
KR20160111869A (ko) | 2016-09-27 |
US20160271913A1 (en) | 2016-09-22 |
CN105985634B (zh) | 2019-11-26 |
KR102357011B1 (ko) | 2022-01-28 |
EP3069871B1 (de) | 2017-07-19 |
RU2016109455A (ru) | 2017-09-21 |
JP2016172447A (ja) | 2016-09-29 |
BR102016005643A2 (pt) | 2018-04-10 |
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