CN115413292A - 用于运输或存储氢的多层结构体 - Google Patents
用于运输或存储氢的多层结构体 Download PDFInfo
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- CN115413292A CN115413292A CN202180028433.6A CN202180028433A CN115413292A CN 115413292 A CN115413292 A CN 115413292A CN 202180028433 A CN202180028433 A CN 202180028433A CN 115413292 A CN115413292 A CN 115413292A
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- multilayer structure
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- polyamide
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 70
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 70
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- 238000009826 distribution Methods 0.000 claims abstract description 6
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Abstract
本发明涉及由包含至少一种聚酰胺的组合物组成的密封层(1)用于制备多核结构体的用途,所述多核结构体旨在用于氢的运输、分配或存储,特别地用于氢的分配或存储,尤其是用于氢的存储,该密封层满足对于氢中存在的和在氢与其接触之后从密封层提取的污染物的测试,该测试按照在标准CSA/ANSI CHMC 2:19中所定义的来进行,在氢中所提取的所述污染物的总比例小于或等于组合物的成分的总和的3重量%,特别地小于2重量%。
Description
技术领域
本专利申请涉及这样的多层结构体:其旨在用于氢(hydrogen,氢气)的运输、分配或存储,特别地用于氢的分配或存储,尤其是用于氢的存储,该多层结构体包含由聚酰胺的组合物构成的密封层,和所述密封层的用途,所述密封层满足对于存在于氢中和被氢从所述密封层提取的污染物的测试,以及其制造方法。
背景技术
氢罐目前吸引了来自众多制造商的广泛关注,尤其是在汽车领域中。寻求的目标之一是提出污染越来越少的车辆。因此,包含电池的电动或混动车辆旨在逐步替代内燃机车辆例如汽油或柴油车辆。事实证明,电池是相对复杂的车辆组件。取决于电池在车辆中的位置,可能需要保护其免受冲击和外部环境的影响,所述外部环境可具有极端温度和可变湿度。还必须避免任何火灾风险。
另外,重要的是其运行温度不超过55℃,以便不破坏电池的单元电池和保持其寿命。相反,例如在冬天,可能需要提高电池温度以优化其运行。
此外,电动车辆如今仍然存在几个问题,即电池续航里程,稀土金属在这些电池中的使用,稀土金属的资源不是无限的,充电时间比加满油箱所用的时间长得多,以及各个国家的电力生产的问题以便能够为电池充电。
因此,氢是电池的替代品,因为氢可通过燃料单元电池转化成电,从而为电动车辆提供动力。
因此,为燃料单元电池供应氢需要存在于车辆中的氢存储罐和用于将氢从罐运输到燃料单元电池的管道两者。
氢罐或氢运输管道通常由必须防止氢渗出的金属或热塑性衬里(或密封层)组成。所设想的罐的类型之一(称为IV型)基于热塑性衬里,复合材料缠绕在该衬里周围。
它们的基本原理是将密封和机械强度这两个基本功能分开,并且彼此独立地管理它们。在这种类型的罐中,由热塑性树脂制成的衬里(或密封护套)与由纤维(玻璃、芳纶、碳)组成的增强结构体(也称为增强护套或层)相结合,其使得可在高得多的压力下运行,同时降低重量并且避免在发生严重外部侵害(attack)的情况下的爆炸性破裂的风险。
对于运输管道而言问题相同。
衬里必须具有某些基本特性:
可通过挤出吹塑模塑、滚塑模塑、注射模塑或挤出进行转化
对氢渗透性低,实际上,衬里的渗透性是限制罐中氢损失的关键因素;
在低温(-40至-70℃)下的机械性质(疲劳)良好;
120℃下热耐受。
然而,燃料单元电池对各种污染物非常敏感,这些污染物降低其性能和其耐用性。
这些污染物可源自多种来源:
由于制造氢的方法而来自氢本身,
来自罐和/或氢运输管道的制造,其中不同的天然成分(例如挥发性有机化合物或水)被捕获在密封层的热塑性聚合物中,并且将随后在氢与所述密封层接触时被氢提取,
来自热塑性聚合物中存在的成分,所述成分能够随后在氢与所述密封层接触时被氢提取。
根据Chen等人(A review of PEM hydrogen fuel cell contamination:impact,mechanisms and mitigation,Journal of Power Sources,165(2007),739-756),在研究、开发和示范中用作燃料单元电池中的燃料的氢主要源自可商购获得的来源。生产氢的方法主要通过以下进行:从烃或含氧烃(包括来自天然气的甲烷和来自生物质的甲醇)重整,以及小有机分子的电解、部分氧化和硼氢化钠的水解。
因此,与燃料单元电池一起使用的氢罐或运输管道不仅必须具有以上所列的基本特征,而且在与所述罐和/或管道的密封层接触之后,氢必须仅含有从所述密封层提取的最小(最少)污染物。
通过提供旨在用于运输、分配或存储氢的本发明的多层结构体,解决了这一双重问题。
在整个该说明书中,术语“衬里”和“密封护套”具有相同的含义。
因此,本发明涉及由包含至少一种聚酰胺的组合物组成的密封层(1)用于制备多层结构体的用途,所述多层结构体旨在用于氢的运输、分配或存储,特别地用于氢的分配或存储,尤其是用于氢的存储,所述密封层满足对于氢中存在的和在氢与其接触之后从密封层提取的污染物的测试,该测试按照在标准CSA/ANSI CHMC 2:19中所定义地来进行,在氢中所提取的所述污染物的总比例小于或等于组合物的成分的总和的3重量%,特别地小于2重量%。
因此,发明人已经发现,由包含至少一种聚酰胺的组合物组成的密封层(1)使得可制备旨在用于氢的运输、分配或存储的多层结构体,其具有以上所列的基本特征,但是还使得可限制氢中存在的和在氢与所述密封层接触之后提取的污染物的比例。
“多层结构体”应理解为包含若干层或由若干层组成的罐,即若干密封层和若干增强层,或一个密封层和若干增强层,或若干密封层和一个增强层或一个密封层和一个增强层。
本发明中的多层结构体还表示旨在用于将氢从罐运输至燃料单元电池的管道或管,并且其包含若干层或由若干层组成,所述若干层即若干密封层和若干外层,或一个密封层和若干外层,或若干密封层和一个外层或一个密封层和一个外层。
表述“所述密封层满足对于氢中存在的和被氢从密封层提取的污染物的测试”意味着氢中存在的和在与氢接触之后源自密封层的污染物的比例,无论其是罐还是管道,都不超过阻止燃料单元电池的正确运行的限值数值。
标准CSA/ANSI CHMC 2:19给出了关于用于确定在使用期间在暴露于氢期间的聚合物的顶部空间中的挥发性组分的程序的详细信息。
表述“在氢与其接触之后”意味着,就像上面一样,在使用期间暴露于氢。
设备
测试设备必须包含以下元件(elements,要素):
a)用于预浓缩气体样品的冷阱;
b)与适当的质量选择检测器串联连接的使用适当的柱的气相色谱仪;
c)顶部空间小瓶(40ml),隔膜,环形封闭件和小瓶的密封件;
d)能够称重最高达60.0001g的分析天平;和
e)能够保持70±5℃的温度的对流烘箱。
测试环境
氢气纯度
氢包装气体必须具有已知的组成和纯度,如下所述。
用于填充测试腔室的氢气的纯度必须至少符合标准ISO 14687:2019,第1至3部分,或SAE J2719(2015)。ISO 14687-2定义了氢的最严格的品质规范,具有在这些ISO标准中对于每种杂质的最低阈值(参见表1)。SAE J2719也适用于具有质子交换膜(PEM)燃料单元电池的车辆,并且与ISO 14687-2一致。
[表1]
*所有值均以ppm(v/v)给出,除非另有说明
测量和仪器
进行氢传输速度测量的温度必须控制在±1℃内。测试压力必须保持恒定在测试值的1%内。
测试程序
测试程序在标准ISO 14687:2019中在第5.6段中描述。
关于污染物
术语污染物以术语的最宽泛的含义被理解为从所述污染物被氢从所述密封层提取的时刻起,并且不是已经存在于被引入到所述多层结构体中以使车辆的燃料单元电池运行的氢中的,例如由于获得氢的方法。
例如,术语污染物涵盖金属阳离子例如K+、Cu2+、Ni2+和Fe3+,其可由在聚酰胺中使用的稳定剂产生,有机或金属稳定剂本身,增塑剂,低聚物,特别是己内酰胺及其环状二聚体1,8-二氮杂环十四烷-2,7-二酮(DCDD),挥发性有机化合物例如NH3,NOx,SOx,N2,苯甲酸化合物,O3,在制造密封层之后被聚酰胺吸收的水,脂肪物质例如油。
因此,挥发性有机化合物不包括以上列表中引用的所有其他材料。
在氢中所提取的所述污染物的总比例小于或等于所述组合物的成分的总和的3重量%,特别地小于2重量%。因此,所述所提取的污染物的总比例不考虑源自制备氢的方法或任何其他来源的污染物的比例。
有利地,在氢中所述所提取的污染物的总比例占0.01重量%至3重量%,特别地0.01重量%至2重量%,更特别地0.01重量%至1重量%,尤其是0.01重量%至0.5重量%。
在第一变体中,所提取的污染物选自增塑剂、稳定剂、低聚物、水、脂肪物质、挥发性有机化合物以及其混合物。
有利地,在该第一变体中,每种单独的所提取的污染物的重量比例小于或等于1%。
在该第一变体的实施方案中,所提取的污染物的构成如下:
最高达1%的增塑剂,
最高达0.5%的稳定剂,
最高达0.5%的低聚物,
最高达0.5%的水,
最高达0.5%的脂肪物质,以及
最高达0.5%的挥发性有机化合物,
所提取的污染物的总和小于或等于所述组合物的成分的总和的3重量%,特别地小于2重量%。
有利地,在该第一变体的该实施方案中,在氢中所述所提取的污染物的总比例占0.01重量%至3重量%,特别地0.01重量%至2重量%,更特别地0.01重量%至1重量%,尤其是0.01重量%至0.5重量%。
更有利地,在该第一变体的该实施方案中,每种单独的所提取的污染物的重量比例小于或等于1%。
在第二变体中,所提取的污染物选自稳定剂、水、油、挥发性有机化合物以及其混合物。
有利地,在该第二变体中,每种单独的所提取的污染物的重量比例小于或等于0.5%。
在该第二变体的实施方案中,所提取的污染物的构成如下:
最高达0.5%的稳定剂,
最高达0.5%的水,
最高达0.5%的脂肪物质,以及
最高达0.5%的挥发性有机化合物,
污染物的总和小于或等于所述组合物的成分的总和的2重量%。
有利地,在该第二变体的该实施方案中,在氢中所述所提取的污染物的总比例占0.01重量%至2重量%,更特别地0.01重量%至1重量%,尤其是0.01重量%至0.5重量%。
更有利地,在该第二变体的该实施方案中,每种单独的所提取的污染物的重量比例小于或等于0.5%。
关于组合物
在第一实施方案中,构成所述密封层(1)的组合物,尤其是在以上定义的第一变体中,包含,按重量计:
至少63.5重量%的聚酰胺,
0至30重量%的冲击改性剂,尤其是0至小于15重量%的冲击改性剂,特别地0至12重量%的冲击改性剂,
0至1.5重量%的增塑剂,以及
0至5重量%的添加剂,
组合物的成分的总和等于100%。
有利地,该第一实施方案的所述组合物包含1至30重量%的冲击改性剂,尤其是1至小于15重量%的冲击改性剂,特别地1至12重量%的冲击改性剂。
有利地,该第一实施方案的所述组合物包含0.1至1.5%的增塑剂。
有利地,该第一实施方案的所述组合物包含0.1至5重量%的添加剂。
有利地,该第一实施方案的所述组合物包含1至30%的冲击改性剂,尤其是1至小于15%的冲击改性剂,特别地1至12%的冲击改性剂和0.1至1.5%的增塑剂。
有利地,该第一实施方案的所述组合物包含1至30重量%的冲击改性剂,尤其是1至小于15重量%的冲击改性剂,特别地1至12重量%的冲击改性剂和0.1至5重量%的添加剂。
有利地,该第一实施方案的所述组合物包含0.1至1.5%的增塑剂和0.1至5重量%的添加剂。
有利地,该第一实施方案的所述组合物包含1至30重量%的冲击改性剂,尤其是1至小于15重量%的冲击改性剂,特别地1至12重量%的冲击改性剂,0.1至1.5%的增塑剂和0.1重量%至5重量%的添加剂。
在第二实施方案中,构成所述密封层(1)的组合物,尤其是在以上定义的第一变体中,由以下组成,按重量计:
至少63.5重量%的聚酰胺,
0至30重量%的冲击改性剂,尤其是0至小于15重量%的冲击改性剂,特别地0至12重量%的冲击改性剂,
0至1.5重量%的增塑剂,以及
0至5重量%的添加剂,
组合物的成分的总和等于100%。
有利地,该第二实施方案的所述组合物包含1至30%的冲击改性剂,尤其是1至小于15%的冲击改性剂,特别地1至12%的冲击改性剂。
有利地,该第二实施方案的所述组合物包含0.1至1.5%的增塑剂。
有利地,该第二实施方案的所述组合物包含0.1至5重量%的添加剂。
有利地,该第二实施方案的所述组合物包含1至小于15%的冲击改性剂,特别地1至12%的冲击改性剂和0.1至1.5%的增塑剂。
有利地,该第二实施方案的所述组合物包含1至小于15重量%的冲击改性剂,特别地1至12重量%的冲击改性剂和0.1至5重量%的添加剂。
有利地,该第二实施方案的所述组合物包含0.1至1.5%的增塑剂和0.1至5重量%的添加剂。
有利地,该第二实施方案的所述组合物包含1至30重量%的冲击改性剂,尤其是1至小于15重量%的冲击改性剂,特别地1至12重量%的冲击改性剂,0.1至1.5%的增塑剂和0.1重量%至5重量%的添加剂。
在第三实施方案中,构成所述密封层(1)的组合物,尤其是在以上定义的第二变体中,包含,按重量计:
至少63.5重量%的聚酰胺,
0至30重量%的冲击改性剂,尤其是0至小于15重量%的冲击改性剂,特别地0至12重量%的冲击改性剂,以及
0至5重量%的添加剂,
组合物的成分的总和等于100%。
有利地,该第三实施方案的所述组合物包含1至30%的冲击改性剂,尤其是1至小于15%的冲击改性剂,特别地1至12%的冲击改性剂。
有利地,该第三实施方案的所述组合物包含0.1至5重量%的添加剂。
有利地,该第三实施方案的所述组合物包含1至30重量%的冲击改性剂,尤其是1至小于15重量%的冲击改性剂,特别地1至12重量%的冲击改性剂和0.1至5重量%的添加剂。
在第四实施方案中,构成所述密封层(1)的组合物,尤其是在以上定义的第二变体中,由以下组成,按重量计:
至少63.5重量%的聚酰胺,
0至30重量%的冲击改性剂,尤其是0至小于15重量%的冲击改性剂,特别地0至12重量%的冲击改性剂,以及
0至5重量%的添加剂,
组合物的成分的总和等于100%。
有利地,该第四实施方案的所述组合物包含1至30%的冲击改性剂,尤其是1至小于15%的冲击改性剂,特别地1至12%的冲击改性剂。
有利地,该第四实施方案的所述组合物包含0.1至5重量%的添加剂。
有利地,该第四实施方案的所述组合物包含1至30重量%的冲击改性剂,尤其是1至小于15重量%的冲击改性剂,特别地1至12重量%的冲击改性剂和0.1至5重量%的添加剂。
关于聚酰胺
用于定义聚酰胺的命名法在ISO标准1874-1:2011"Plastiques--Matériauxpolyamides(PA)pour moulage et extrusion--Partie 1:Désignation"中,尤其是在第3页(表1和2)中描述并且为本领域技术人员所熟知。
聚酰胺可为均聚酰胺或共聚酰胺或其混合物。
聚酰胺是半结晶聚合物,也就是说,是这样的材料:其在环境温度下通常是固体,并且在温度升高期间,特别地在通过其玻璃化转变温度(Tg)之后软化,并且可在通过所谓的其熔点(Tm)时表现出急剧的转变,并且当温度降低至其结晶温度以下时,其再次变为固体。
Tg、Tc和Tm分别根据标准11357-2:2013和11357-3:2013通过差示扫描量热法(DSC)测定。
所述半结晶聚酰胺的数均分子量Mn优选在10,000至85,000、尤其是10,000至60,000、优先地10,000至50,000、甚至更优先地12,000至50,000的范围内。这些Mn值可对应于大于或等于0.8的特性粘度,如根据标准ISO 307:2007在间甲酚中但是通过改变溶剂(使用间甲酚代替硫酸,以及温度为20℃)测定。
在一个实施方案中,聚酰胺选自脂族聚酰胺、半芳族聚酰胺和两者的混合物,有利地脂族聚酰胺。
所述脂族聚酰胺可源自以下的缩聚:
至少一种C6至C18、优先地C9至C18、更优先地C10至C18、甚至更优先地C10至C12、特别地C11氨基酸;或
至少一种C6至C18、优先地C9至C18、更优先地C10至C18、甚至更优先地C10至C12、特别地C12内酰胺;或
至少一种C4至C36、特别地C6至C36、优先地C6至C18、优先地C6至C12、更优先地C10至C12Ca脂族二胺与至少一种C4至C36、特别地C6至C36、优先地C6至C18、优先地C10至C18、更优先地C10至C12 Cb脂族二胺。
C6至C12氨基酸特别地是6-氨基己酸、9-氨基壬酸、10-氨基癸酸、10-氨基十一烷酸、12-氨基十二烷酸和11-氨基十一烷酸以及其衍生物,尤其是N-庚基-11-氨基十一烷酸。
当所述至少一种半结晶脂族聚酰胺由至少一种内酰胺的缩聚获得时,其可因此包含单一氨基酸或若干氨基酸。
有利地,所述半结晶脂族聚酰胺由单一氨基酸的缩聚获得并且所述氨基酸选自11-氨基十一烷酸和12-氨基十二烷酸,有利地11-氨基十一烷酸。
C6至C12内酰胺尤其是己内酰胺、癸内酰胺、十一内酰胺和月桂基内酰胺。
当所述至少一种半结晶脂族聚酰胺由至少一种内酰胺的缩聚获得时,其可因此包含单一内酰胺或若干内酰胺。
有利地,所述至少一种半结晶脂族聚酰胺由单一内酰胺的缩聚获得,并且所述内酰胺选自月桂基内酰胺和十一内酰胺,有利地月桂基内酰胺。
Ca二胺可为直链或支链的。有利地,其为直链的。
所述至少一种C4-C36 Ca二胺可特别地选自:丁烷亚甲基二胺、1,5-五亚甲基二胺、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、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、1,13-十三亚甲基二胺、1,14-十四亚甲基二胺、1,16-十六亚甲基二胺和1,18-十八亚甲基二胺、十八碳烯二胺、二十烷二胺、二十二烷二胺和由脂肪酸获得的二胺。
有利地,所述至少一种C6-C36 Ca二胺选自: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、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、1,13-十三亚甲基二胺、1,14-十四亚甲基二胺、1,16-十六亚甲基二胺和1,18-十八亚甲基二胺、十八碳烯二胺、二十烷二胺、二十二烷二胺和由脂肪酸获得的二胺。
所述至少一种C4至C36二羧酸Cb可选自丁二酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、十一烷二酸、十二烷二酸、十三烷二酸、十四烷二酸、十五烷二酸、十六烷二酸、十八烷二酸和由脂肪酸获得的二酸。
二酸可为直链或支链的。有利地,其为直链的。
有利地,脂族聚酰胺选自PA6、PA66、PA11、PA12、PA610、PA612、PA1010、PA1012和PA1212。
所述半芳族聚酰胺可尤其为如下的半芳族聚酰胺:其具有式X/YAr,如EP1505099中所述,尤其是具有式A/XT的半芳族聚酰胺,其中A选自从如前文所定义的氨基酸获得的单元、从如前文所定义的内酰胺获得的单元和对应于式(Cc二胺).(Cd二酸)的单元,其中c代表二胺的碳原子数并且d代表二酸的碳原子数,c和d各自在4和36之间,有利地在9和18之间,(Cc二胺)单元选自如前文所定义的直链或支链脂族二胺、脂环族二胺和烷基芳族二胺,并且(Cd二酸)单元选自如前文所定义的直链或支链脂族二酸、脂环族二酸和芳族二酸;
X.T表示从Cx二胺和对苯二甲酸的缩聚获得的单元,其中x代表Cx二胺的碳原子数,x在5和36之间,有利地在9和18之间,尤其是具有式A/5T、A/6T、A/9T、A/10T或A/11T的聚酰胺,A如上所定义,特别是选自以下的聚酰胺:PA MPMDT/6T,PA11/10T,PA 5T/10T,PA 11/BACT,PA 11/6T/10T,PA MXDT/10T,PA MPMDT/10T,PA BACT/10T,PA BACT/6T,PA BACT/10T/6T,PA 11/BACT/6T,PA 11/MPMDT/6T,PA 11/MPMDT/10T,PA 11/BACT/10T,PA 11/MXDT/10T,11/5T/10T。
T对应于对苯二甲酸,MXD对应于间苯二甲二胺,MPMD对应于甲基五亚甲基二胺并且BAC对应于双(氨基甲基)环己烷。
所述半芳族聚酰胺也可为具有式ZAr的聚酰胺,其中Z是从如前文所定义的至少一种Ca脂族二胺的缩聚获得的单元,并且Ar是芳族二羧酸,特别地对苯二甲酸、间苯二甲酸和萘酸。
在一个实施方案中,聚酰胺是脂族的并且选自PA6、PA66、PA11、PA12、PA610、PA612、PA1010、PA1012和PA1212。
在另一个实施方案中,聚酰胺是半芳族的并且选自聚酰胺11/5T、11/6T、11/10T、MXDT/10T、MPMDT/10T和BACT/10T。
在一个实施方案中,所述组合物的所述聚酰胺先前用选自极性溶剂(特别是甲醇、水或水蒸气,或其混合物)的体系洗涤至少一次。
关于冲击改性剂
冲击改性剂可为任何冲击改性剂,只要它是具有在树脂的模量以下的模量、具有良好的对基质的粘附的聚合物,从而耗散开裂能量。
冲击改性剂有利地由如下的聚合物组成:所述聚合物具有根据标准ISO178测量的在100Mpa以下的弯曲模量和在0℃以下的Tg(根据标准11357-2在DSC热谱图的拐点处测量),特别是聚烯烃。
在一个实施方案中,PEBA从冲击改性剂的定义中排除。
冲击改性剂的聚烯烃可为官能化的或非官能化的,或者为至少一种官能化聚烯烃和/或至少一种非官能化聚烯烃的混合物。为了简化,聚烯烃表示为(B)并且官能化聚烯烃(B1)和非官能化聚烯烃(B2)如下所述。
非官能化聚烯烃(B2)经典地是α-烯烃或二烯烃(例如乙烯、丙烯、1-丁烯、1-辛烯、丁二烯)的均聚物或共聚物。例如,可提及:
-聚乙烯的均聚物和共聚物,特别是LDPE、HDPE、LLDPE(线性低密度聚乙烯)、VLDPE(极低密度聚乙烯)和茂金属聚乙烯。
-丙烯的均聚物或共聚物。
-乙烯/α-烯烃共聚物例如乙烯/丙烯、EPR(乙烯-丙烯-橡胶的缩写)和乙烯/丙烯/二烯(EPDM)。
-苯乙烯/乙烯-丁烯/苯乙烯(SEBS)、苯乙烯/丁二烯/苯乙烯(SBS)、苯乙烯/异戊二烯/苯乙烯(SIS)、苯乙烯/乙烯-丙烯/苯乙烯(SEPS)嵌段共聚物。
-乙烯与选自不饱和羧酸的盐或酯例如(甲基)丙烯酸烷基酯(例如丙烯酸甲酯)或饱和羧酸的乙烯酯例如乙酸乙烯酯(EVA)的至少一种产物的共聚物,共聚单体的比例能够达到40重量%。
官能化聚烯烃(B1)可为具有反应性单元(官能团)的α-烯烃的聚合物;这样的反应性单元是酸、酸酐或环氧官能团。举例来说,可提及前述的聚烯烃(B2),其被以下接枝或共聚或三元共聚:不饱和环氧化物例如(甲基)丙烯酸缩水甘油酯,或者羧酸或相应的盐或酯例如(甲基)丙烯酸(其可完全或部分地被金属例如锌等中和),或者甚至羧酸酐例如马来酸酐。官能化聚烯烃为例如PE/EPR混合物,其重量比率可宽泛地变化,例如在40/60和90/10之间,所述混合物用酸酐、尤其是马来酸酐共接枝,符合例如0.01至5重量%的接枝率。
所述官能化聚烯烃(B1)可选自以下的马来酸酐或甲基丙烯酸缩水甘油酯接枝的(共)聚合物,其中接枝率为例如0.01至5重量%:
-PE,PP,乙烯与丙烯、丁烯、己烯或辛烯的共聚物,含有例如35至80重量%的乙烯;
-乙烯/α-烯烃共聚物例如乙烯/丙烯、EPR(乙烯-丙烯-橡胶的缩写)和乙烯/丙烯/二烯(EPDM)。
-苯乙烯/乙烯-丁烯/苯乙烯(SEBS)、苯乙烯/丁二烯/苯乙烯(SBS)、苯乙烯/异戊二烯/苯乙烯(SIS)、苯乙烯/乙烯-丙烯/苯乙烯(SEPS)嵌段共聚物。
-乙烯和乙酸乙烯酯共聚物(EVA),含有最高达40重量%的乙酸乙烯酯;
-乙烯和(甲基)丙烯酸烷基酯共聚物,含有最高达40重量%的(甲基)丙烯酸烷基酯;
-乙烯和乙酸乙烯酯(EVA)和(甲基)丙烯酸烷基酯共聚物,含有最高达40重量%的共聚单体。
官能化聚烯烃(B1)也可选自乙烯/丙烯共聚物,具有主要马来酸酐接枝的丙烯,然后与单胺聚酰胺(或聚酰胺低聚物)缩合(EP-A-0342066中描述的产物)。
官能化聚烯烃(B1)也可为至少以下单元的共聚物或三元共聚物:(1)乙烯,(2)(甲基)丙烯酸烷基酯或饱和羧酸的乙烯基酯和(3)酸酐例如马来酸酐或(甲基)丙烯酸或环氧树脂例如(甲基)丙烯酸缩水甘油酯。
作为后一种类型的官能化聚烯烃的实例,可提及以下共聚物,其中乙烯优选占至少60重量%并且其中三元共聚单体(官能(function))占例如共聚物的0.1至10重量%:
-乙烯/(甲基)丙烯酸烷基酯/(甲基)丙烯酸或马来酸酐或甲基丙烯酸缩水甘油酯共聚物;
-乙烯/乙酸乙烯酯/马来酸酐或甲基丙烯酸缩水甘油酯共聚物;
-乙烯/乙酸乙烯酯或(甲基)丙烯酸烷基酯/(甲基)丙烯酸或马来酸酐或甲基丙烯酸缩水甘油酯共聚物。
在前述共聚物中,(甲基)丙烯酸可用Zn或Li盐化。
(B1)或(B2)中的术语“(甲基)丙烯酸烷基酯”表示甲基丙烯酸C1至C8烷基酯和丙烯酸C1至C8烷基酯,并且可选自丙烯酸甲酯、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、丙烯酸环己酯、甲基丙烯酸甲酯和甲基丙烯酸乙酯。
而且,前面引用的聚烯烃(B1)也可通过任何适当的方法或试剂(二环氧基、二酸、过氧化物等)交联;术语官能化聚烯烃还包括前面引用的聚烯烃与可与这些反应的二官能试剂(例如二酸、二酐、二环氧基等)的混合物,或可一起反应的至少两种官能化聚烯烃的混合物。
以上提及的共聚物(B1)和(B2)可以统计或有序的方式共聚,并且具有直链或支链结构。
这些聚烯烃的分子量、指数MFI、密度也可宽泛地变化,这是本领域技术人员将知道的。MFI(熔体流动指数(Melt Flow Index)的缩写)是熔融状态下的流动性的量度。其根据标准ASTM 1238进行测量。
有利地,非官能化聚烯烃(B2)选自聚丙烯的均聚物或共聚物和任何乙烯均聚物或乙烯和更高级α-烯烃共聚单体(例如丁烯、己烯、辛烯或4-甲基-1-戊烯)的共聚物。例如,可提及PP、高密度PE、中密度PE、线性低密度PE、低密度PE、极低密度PE。本领域技术人员已知,这些聚乙烯是根据“自由基”方法、根据“Ziegler”催化方法或更近期的所谓“茂金属”催化作用生产的。
有利地,官能化聚烯烃(B1)选自包含α-烯烃单元和带有极性反应性官能团(例如环氧基、羧酸或羧酸酐官能团)的单元的任何聚合物。作为这样的聚合物的实例,可提及乙烯、烷基丙烯酸酯、和马来酸酐或甲基丙烯酸缩水甘油酯的三元共聚物,如来自申请人的被马来酸酸酐接枝的聚烯烃,如来自申请人的以及乙烯、烷基丙烯酸酯和(甲基)丙烯酸的三元共聚物。还可提及被羧酸酐接枝然后与聚酰胺或单胺聚酰胺低聚物缩合的聚丙烯的均聚物或共聚物。
有利地,构成所述密封层的所述组合物不含聚醚嵌段酰胺(PEBA)。因此,在该实施方案中,PEBA从冲击改性剂中排除。
有利地,所述透明组合物不含核-壳颗粒或核-壳聚合物。
核-壳颗粒必须理解为第一层形成核并且第二层或所有后续层形成相应壳的颗粒。
核-壳颗粒可通过包含至少两个步骤的若干步骤的方法获得。这样的方法例如在文献US2009/0149600或EP0,722961中描述。
在一个实施方案中,当组合物的聚酰胺是半芳族聚酰胺时,冲击改性剂的比例则为0重量%至小于10重量%,尤其是0重量%至8重量%,特别地1重量%至小于10重量%,尤其是从1重量%至8重量%。
有利地,在该最后一个实施方案中,所述组合物还包含0.1至5重量%的添加剂。
关于增塑剂:
增塑剂可为通常用于基于聚酰胺的组合物中的增塑剂。
有利地,使用具有良好的热稳定性的增塑剂,使得在混合不同聚合物和转化所获得的组合物的步骤期间不形成烟雾(fume)。
特别地,该增塑剂可选自:
苯磺酰胺衍生物,例如正丁基苯磺酰胺(BBSA),乙基甲苯磺酰胺(ETSA)、N-环己基甲苯磺酰胺和N-(2-羟丙基)苯磺酰胺的邻位和对位异构体,
羟基苯甲酸的酯,例如对羟基苯甲酸2-乙基己酯(EHPB)和对羟苯甲酸2-癸基己酯,
四氢糠醇的酯或醚,例如低聚亚乙基氧基四氢糠醇,以及
柠檬酸或羟基丙二酸的酯,例如低聚亚乙基氧基丙二酸酯。
优选的增塑剂为正丁基苯磺酰胺(BBSA)。
另一种更特别优选的增塑剂是N-(2-羟丙基)苯磺酰胺(HP-BSA)。实际上,后者具有的优点是防止在通过挤出进行的转化步骤期间在挤出螺杆和/或模具处形成沉积物(“模具口水(die drool)”)。
当然,可使用增塑剂的混合物。
关于添加剂
添加剂可选自抗氧化剂、热稳定剂、UV吸收剂、光稳定剂、润滑剂、无机填料、阻燃剂、成核剂和染料。
关于结构体
根据另一方面,本发明涉及多层结构体,其包含如前文所定义的至少一个密封层(1)。
在氢与所述密封层的接触期间,氢中提取和存在的所述污染物的总比例小于或等于构成所述密封层的组合物的成分的总和的3重量%,特别地小于的2重量%,根据标准CSA/ANSI CHMC 2:19中定义的测试确定。
在第一实施方案中,所述多层结构体对应于罐,并且进一步包含至少一个复合增强层(2),所述密封层与氢接触。
第一实施方案:罐
因此,所述多层结构体可包含至少一个密封层和缠绕在密封层周围的并且可或可不彼此粘附的至少一个复合增强层。
在一个实施方案中,所述复合增强层(2)中的至少一个由呈连续纤维形式的纤维质材料组成,所述连续纤维浸渍有主要包含至少一种聚合物P2j(j=1至m,m是增强层的数量)(特别是环氧化物树脂或基于环氧化物的树脂)的组合物,
所述结构体不含最外层并且与聚酰胺聚合物复合增强体的最外层相邻。
有利地,所述密封层和增强层不相互粘附,并且由分别包含不同聚合物的组合物组成。
然而,所述不同聚合物可为相同类型的。
因此,如果两个复合增强和密封层中的一个由包含脂族聚酰胺的组合物制成,则另一个层由包含为非脂族的并且为例如半芳族聚酰胺的聚酰胺的组合物制成,以便具有高Tg聚合物作为复合增强材料的基质。
所述多层结构可包含不同性质的最高达10个密封层和最高达10个复合增强层。
显然,所述多层结构体不一定是对称的,并且因此它可包含比复合层更多的密封层,或反之亦然,但不可有层和增强层的交替。
有利地,所述多层结构体包含一个、两个、三个、四个、五个、六个、七个、八个、九个或十个密封层以及一个、两个、三个、四个、五个、六个、七个、八个、九个或十个复合增强层。
有利地,所述多层结构体包含一个、两个、三个、四个或五个密封层以及一个、两个、三个、四个或者五个复合增强层。
有利地,所述多层结构体包含一个、两个或三个密封层以及一个、两个或三个复合增强层。
在一个实施方案中,所述多层结构体包含单一密封层和若干增强层,所述相邻增强层缠绕在所述密封层周围并且其他增强层缠绕在直接相邻的增强层周围。
在另一个实施方案中,所述多层结构体包含单一增强层和若干密封层,所述增强层缠绕在所述相邻密封层周围。
在一个有利的实施方案中,所述多层结构体包含单一密封层和单一复合增强层,所述增强层缠绕在所述密封层周围。
因此,这两层的所有组合都在本发明的范围内,条件是,至少所述最内复合增强层缠绕在所述最外相邻密封层周围,其他层彼此粘附或不彼此粘附。
有利地,在所述多层结构体中,每个密封层由包含相同类型的聚酰胺的组合物组成。
表述“相同类型的聚合物”意指,例如,聚酰胺,其可为相同的聚酰胺或不同的聚酰胺,这取决于诸层。
有利地,在所述多层结构体中,每个增强层由包含相同类型的聚合物P2j(特别是环氧树脂或基于环氧的树脂)的组合物组成。
有利地,在所述多层结构体中,每个密封层包含相同类型的聚酰胺,并且每个增强层包含相同类型的聚合物P2j,特别是环氧化物树脂或基于环氧化物的树脂。
有利地,聚酰胺P2j对于所有增强层都是相同的。
有利地,所述聚合物P2j为环氧化物树脂或基于环氧化物的树脂。
有利地,聚酰胺对于所有密封层都是相同的。
有利地,密封层的所述聚酰胺是脂族聚酰胺,特别是PA6,PA66,PA610,PA612,PA1010,PA 1012,PA 1212,PA11,PA12,尤其是PA 11或PA12,并且所述聚合物P2j为半芳族聚酰胺,特别地选自:PA MPMDT/6T,PA11/10T,PA 11/BACT,PA 5T/10T,PA 11/6T/10T,PAMXDT/10T,PA MPMDT/10T,PA BACT/10T,PA BACT/6T,PA BACT/10T/6T,PA 11/BACT/6T,PA11/MPMDT/6T,PA 11/MPMDT/10T,PA 11/BACT/10T,PA和11/MXDT/10T。
在一个实施方案中,所述多层结构体由单一增强层和单一密封层组成,其中密封层的所述聚酰胺是长链脂族聚酰胺,特别是PA1010,PA 1012,PA 1212,PA11,PA12,尤其是PA 11或PA12,并且所述聚合物P2j为半芳族聚酰胺,特别地选自:PA MPMDT/6T,PA11/10T,PA 11/BACT,PA 5T/10T,PA 11/6T/10T,PA MXDT/10T,PA MPMDT/10T,PA BACT/10T,PABACT/6T,PA BACT/10T/6T,PA 11/BACT/6T,PA 11/MPMDT/6T,PA 11/MPMDT/10T,PA 11/BACT/10T,和PA 11/MXDT/10T。
长链聚酰胺是具有大于8的每个氮原子的平均碳原子数的聚酰胺。
在另一个实施方案中,所述多层结构体由单一增强层和单一密封层组成,其中密封层(1)的所述聚酰胺是长链脂族聚酰胺,特别是PA1010,PA 1012,PA 1212,PA12,尤其是PA 12,并且所述聚合物P2j为半芳族聚酰胺,特别地选自:PA MPMDT/6T,PA PA11/10T,PA11/BACT,PA 5T/10T,PA 11/6T/10T,PA MXDT/10T,PA MPMDT/10T,PA BACT/10T,PA BACT/6T,PA BACT/10T/6T,PA 11/BACT/6T,PA 11/MPMDT/6T,PA 11/MPMDT/10T,PA 11/BACT/10T和PA 11/MXDT/10T。
在又一个实施方案中,多层结构体由单一增强层和单一密封层组成,其中密封层(1)的所述聚酰胺是长链脂族聚酰胺,特别是PA1010,PA 1012,PA 1212,PA11,PA12,或半芳族聚酰胺,特别地选自聚酰胺11/5T或11/6T或11/10T,MXDT/10T,MPMDT/10T和BACT/10T,特别是PA11或PA12,并且所述聚合物P2j为环氧化物或基于环氧化物的树脂。
在另一个实施方案中,多层结构体由单一增强层和单一密封层组成,其中密封层(1)的所述聚酰胺是长链脂族聚酰胺,特别是PA1010,PA 1012,PA 1212,PA12,或半芳族聚酰胺,特别地选自聚酰胺11/5T或11/6T或11/10T,MXDT/10T,MPMDT/10T和BACT/10T,特别是PA12,并且所述聚合物P2j为环氧化物或基于环氧化物的树脂。
有利地,所述多层结构体进一步包含至少一个由纤维质材料组成的外层,该纤维质材料由浸有透明无定形聚合物的连续玻璃纤维制成,所述层是所述多层结构体的最外层。
所述外层是第二增强层,但是是透明的,这使得可在结构体上放置文本。
在第二实施方案中,所述多层结构体对应于管道,并且进一步包含至少一个外金属编织体(2’),所述密封层与氢接触。
因此,在最后一个实施方案中没有复合增强层。
该管道尤其旨在用于将前文定义的罐连接至燃料单元电池。
密封层的特征与上述相同。
关于纤维质材料
关于构成所述纤维质材料的纤维,它们特别是矿物、有机或植物纤维。
有利地,所述纤维质材料可为上浆(sized)或未上浆的。
因此,所述纤维质材料可包含最高达3.5重量%的有机材料(热固性或热塑性树脂类型),称为上浆。
矿物纤维包括例如碳纤维、玻璃纤维、玄武岩或基于玄武岩的纤维、二氧化硅纤维或碳化硅纤维。有机纤维包括基于热塑性或热固性聚合物的纤维,例如半芳族聚酰胺纤维、芳族聚酰胺纤维或聚烯烃纤维。优选地,它们是基于无定形热塑性聚合物的,并且具有高于构成预浸渍基体的聚合物或热塑性聚合物混合物的Tg的玻璃化转变温度Tg(当聚合物或热塑性聚合物混合物是无定形的时),或者高于构成预浸渍基体的聚合物或热塑性聚合物混合物的Tm的玻璃化转变温度Tg(当聚合物或热塑性聚合物混合物是半结晶的时)。有利地,它们是基于半结晶热塑性聚合物的,并且具有高于构成预浸渍基体的聚合物或热塑性聚合物混合物的Tg的熔化温度Tm(当聚合物或热塑性聚合物混合物是无定形的时),或者高于构成预浸渍基体的聚合物或热塑性聚合物混合物的Tm的熔化温度Tm(当聚合物或热塑性聚合物混合物是半结晶的时)。因此,在被最终复合物的热塑性基体浸渍期间,构成纤维质材料的有机纤维没有熔化风险。植物纤维包括天然亚麻、火麻(hemp,汉麻)、木质素、竹子、丝、特别是蜘蛛丝、剑麻和其他基于纤维素的纤维,特别是基于粘胶的。这些植物纤维可以纯的方式使用、经处理或涂有涂层,以促进热塑性聚合物基体的粘附和浸渍。
纤维质材料也可为用纤维编织或织造的织物。
其也可对应于具有支撑线的纤维。
这些组分纤维可单独使用或混合使用。因此,有机纤维可与待用热塑性聚合物粉末预浸渍并且形成预浸渍的纤维质材料的矿物纤维混合。
有机纤维束可具有若干克重。它们可进一步具有若干几何形状。纤维质材料的组分纤维可进一步采用这些具有不同几何形状的增强纤维的混合物的形式。纤维是连续纤维。
优选地,纤维质材料选自玻璃纤维,碳纤维,玄武岩纤维或基于玄武岩的纤维,或其混合物,特别是碳纤维。
其以一股或若干股的形式使用。
根据另一方面,本发明涉及一种制造如上所定义的多层结构体的方法,其特征在于,其包括通过注射、挤出、挤出吹塑或旋转模塑制造如权利要求1至12中的一项所定义的密封层(1)的步骤。
在一个实施方案中,所述方法包括用选自极性溶剂(特别是甲醇、水或水蒸气,或其混合物)的体系洗涤组合物的聚酰胺至少一次的先前步骤。
有利地,对应于罐并且如上所定义的多层结构体的制造方法的特征在于,它包括在密封层(1)周围丝缠绕如上所定义的增强层(2)的步骤。
有利地,所述多层结构体在制造之后可用选自极性溶剂(特别是甲醇、水或水蒸气,或其混合物)的体系洗涤至少一次。
在制造之后用极性溶剂(特别是甲醇)或用水/极性溶剂混合物洗涤的情形中,有必要清洗结构体,以完全除去任何痕量的甲醇。
有利地,在制造之后或在制造和洗涤之后,将结构体在干燥空气流下干燥2天,尤其是在40℃至80℃、特别是50℃至70℃的温度下,尤其是在60℃下。
以上详述的所有特征也适用于本方法。
实施例:
以下组合物是根据本领域技术人员熟知的用于本发明的结构体的密封层(1)的组合物的技术制备的(表2)。
[表2]
组合物 | I1 | I2 | I3 | I4 | I5 | C1 | C2 |
PA11 | 100% | 99.7% | 90% | 89.7% | 86% | ||
PA11/10T | 70% | 65% | |||||
增塑剂 | 0 | 0% | 0 | 0 | 0 | 13% | 10% |
冲击改性剂 | 0% | 30% | 0% | 10% | 10% | 0% | 35% |
添加剂 | 0% | 0% | 0.3% | 0% | 0.3% | 0% | 0% |
I1至I2:本发明的组合物
C1至C2:对比组合物
PA11:PA11是具有45,000的Mn(数均分子量)的聚酰胺11。熔化温度为190℃;其熔化焓为56J/g。
PA11/10T:Rilsan HT(Arkema)
增塑剂:BBSA(正丁基苯磺酰胺)
添加剂:稳定剂
包含密封层(1)的本发明的密封层(衬里)通过在适合于所使用的热塑性树脂的性质的温度下,用上述各种组合物旋转模塑密封层(衬里)而获得。
包含由环氧化物树脂或基于环氧化物的树脂制成的复合增强体的多层结构体是通过湿法丝缠绕方法获得的,所述方法由将碳纤维缠绕在衬里周围组成,该纤维已预先在液体环氧化物浴或基于液体环氧化物的浴中预浸渍。然后将罐在烘箱中聚合2小时。
根据标准CSA/ANSI CHMC 2:19,对从由上述组合物制造的多层结构体的各个密封层提取在氢中的污染物进行量化:
具有基于组合物-I1的密封层的多层结构体:<0.5%
具有基于组合物-I2的密封层的多层结构体:<0.5%
具有基于组合物-I3的密封层的多层结构体:<0.5%
具有基于组合物-I4的密封层的多层结构体:<0.5%
具有基于组合物-I5的密封层的多层结构体:<0.5%
具有基于组合物-C1的密封层的多层结构体:>3%
具有基于组合物-C2的密封层的多层结构体:>3%。
Claims (24)
1.由包含至少一种聚酰胺的组合物组成的密封层(1)用于制备多层结构体的用途,所述多层结构体旨在用于氢的运输、分配或存储,特别地用于氢的分配或存储,尤其是用于氢的存储,所述密封层满足对于氢中存在的和在氢与其接触之后从所述密封层提取的污染物的测试,所述测试按照在标准CSA/ANSI CHMC 2:19中所定义地来进行,在氢中所提取的所述污染物的总比例小于或等于所述组合物的成分的总和的3重量%,特别地小于2重量%。
2.根据权利要求1所述的用途,其中所提取的污染物选自增塑剂、稳定剂、低聚物、水、脂肪物质、挥发性有机化合物以及其混合物。
3.根据权利要求2所述的用途,其中每种所提取的单独的污染物的重量比例小于或等于1%。
4.根据权利要求2或3所述的用途,其中所提取的污染物的组成如下:
最高达1%的增塑剂,
最高达0.5%的稳定剂,
最高达0.5%的低聚物,
最高达0.5%的水,
最高达0.5%的脂肪物质,以及
最高达0.5%的挥发性有机化合物,
所提取的污染物的总和小于或等于所述组合物的成分的总和的3重量%,特别地小于2重量%。
5.根据权利要求1至4中的一项所述的用途,其中所述组合物包含以下,按重量计:
至少63.5重量%的聚酰胺,
0至小于30重量%的冲击改性剂,尤其是0至小于15重量%的冲击改性剂,特别地0至12重量%的冲击改性剂,
0至1.5重量%的增塑剂,以及
0至5重量%的添加剂,
组合物的成分的总和等于100%。
6.根据权利要求1所述的用途,其中所提取的污染物选自稳定剂、水、油、挥发性有机化合物以及其混合物。
7.根据权利要求6所述的用途,其中每种所提取的单独的污染物的重量比例小于或等于0.5%。
8.根据权利要求6或7所述的用途,其中所提取的污染物的组成如下:
最高达0.5%的稳定剂,
最高达0.5%的水,
最高达0.5%的脂肪物质,以及
最高达0.5%的挥发性有机化合物,
污染物的总和小于或等于所述组合物的成分的总和的2重量%。
9.根据权利要求6至8中的一项所述的用途,其中所述组合物包含,按重量计:
至少63.5重量%的聚酰胺,
0至小于30重量%的冲击改性剂,尤其是0至小于15重量%的冲击改性剂,特别地0至12重量%的冲击改性剂,以及
0至5重量%的添加剂,
组合物的成分的总和等于100%。
10.根据权利要求1至9中的一项所述的用途,其中聚酰胺选自脂族聚酰胺、半芳族聚酰胺以及其混合物。
11.根据权利要求10所述的用途,其中聚酰胺是脂族的并且选自PA6、PA66、PA11、PA12、PA610、PA612、PA1010、PA1012和PA1212。
12.根据权利要求10所述的用途,其中聚酰胺是半芳族的并且选自聚酰胺11/5T、11/6T、11/10T、MXDT/10T、MPMDT/10T和BACT/10T。
13.多层结构体,其包含至少一个如权利要求1至12中的一项中所定义的密封层(1)。
14.根据权利要求13所述的多层结构体,其特征在于其对应于罐,并且进一步包含至少一个复合增强层(2),所述密封层与氢接触。
15.根据权利要求13或14所述的多层结构体,其特征在于所述复合增强层(2)中的至少一个由呈连续纤维形式的纤维质材料组成,所述连续纤维浸渍有主要包含至少一种聚合物P2j(j=1至m,m是增强层的数量)、特别是环氧化物树脂或基于环氧化物的树脂的组合物,
所述结构体不含最外层并且与聚酰胺聚合物复合增强体的最外层相邻。
16.根据权利要求13至15中的一项所述的多层结构体,其特征在于每个密封层包含相同类型的聚酰胺。
17.根据权利要求13至16中的一项所述的多层结构体,其特征在于每个增强层包含相同类型的聚合物,特别是环氧化物树脂或基于环氧化物的树脂。
18.根据权利要求13至17所述的多层结构体,其特征在于每个密封层包含相同类型的聚酰胺,并且每个增强层包含相同类型的聚合物,特别是环氧化物树脂或基于环氧化物的树脂。
19.根据权利要求13至18中的一项所述的多层结构体,其特征在于其具有单一密封层和单一增强层。
20.根据权利要求13至19中的一项所述的多层结构体,其特征在于所述结构体进一步包含至少一个由纤维质材料组成的外层(3),该纤维质材料由浸有透明无定形聚合物的连续玻璃纤维制成,所述层是所述多层结构体的最外层。
21.根据权利要求13所述的多层结构体,其特征在于其对应于管道,并且进一步包含至少一个外金属编织体(2’),所述密封层与氢接触。
22.如权利要求13至20中的一项中所定义的多层结构体的制造方法,其特征在于其包括通过注射、挤出、挤出吹塑或旋转模塑制造如权利要求1至12中的一项所定义的密封层(1)的步骤。
23.根据权利要求22所述的多层结构体的制造方法,其特征在于其包括在通过注射、挤出或旋转模塑制造所述密封层(1)的步骤之前,用选自极性溶剂,特别是甲醇、水或水蒸气,或其混合物的体系洗涤组合物的聚酰胺至少一次的先前步骤。
24.根据权利要求22或23所述的多层结构体的制造方法,其特征在于其包括在密封层(1)周围丝缠绕如权利要求14至20中的一项中所定义的增强层(2)的步骤。
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