CN109790377B - 具有单层衬里的复合材料压力容器 - Google Patents

具有单层衬里的复合材料压力容器 Download PDF

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Publication number
CN109790377B
CN109790377B CN201780061744.6A CN201780061744A CN109790377B CN 109790377 B CN109790377 B CN 109790377B CN 201780061744 A CN201780061744 A CN 201780061744A CN 109790377 B CN109790377 B CN 109790377B
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polymer composition
liner
pressure vessel
weight
composite pressure
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CN109790377A (zh
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B·克里尔
皮埃尔·德凯泽
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France Quannai Plastic New Energy Co
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France Quannai Plastic New Energy Co
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Priority claimed from EP16192469.1A external-priority patent/EP3275939A1/en
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
    • F17C1/16—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge constructed of plastics materials
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/50—General aspects of joining tubular articles; General aspects of joining long products, i.e. bars or profiled elements; General aspects of joining single elements to tubular articles, hollow articles or bars; General aspects of joining several hollow-preforms to form hollow or tubular articles
    • B29C66/51—Joining tubular articles, profiled elements or bars; Joining single elements to tubular articles, hollow articles or bars; Joining several hollow-preforms to form hollow or tubular articles
    • B29C66/54—Joining several hollow-preforms, e.g. half-shells, to form hollow articles, e.g. for making balls, containers; Joining several hollow-preforms, e.g. half-cylinders, to form tubular articles
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Abstract

提出一种复合材料压力容器，其包括单层衬里和布置在所述衬里上的增强结构，所述衬里通过注射模制制成，所述衬里包括至少两个可焊接在一起的壳体。每个壳体由聚合物组合物制成，所述聚合物组合物包括相对于所述聚合物组合物的总重量的重量比至少为45％的芳香族聚酰胺和相对于所述聚合物组合物的总重量的重量比至少为10％的脂肪族聚酰胺。

Description

具有单层衬里的复合材料压力容器
技术领域
本发明涉及一种用于复合材料压力容器的衬里。特别地，本发明涉及用于存储氢气的非金属衬里。
背景技术
一些车辆使用压缩气体、尤其是氢气作为燃料。这样的车辆一般配备有复合材料压力容器。复合材料压力容器一般包括用于存储氢气的衬里。例如，围绕着衬里施加外部的线缠绕。该线缠绕的形式可以是围绕着衬里的外部缠绕的碳纤维线复合材料。
金属和非金属的两种衬里都有使用，但非金属衬里由于它们的重量较轻而更为优选。
非金属衬里可以是单层类型或多层类型的。
单层类型的衬里一般包括单层聚酰胺。一般使用PA-6。这些已知的衬里的一个缺点在于它们具有大的厚度(通常大于4mm)，以符合与它们的设计用途类型和它们必须满足的环境要求有关的渗透性标准。这增加了压力容器的重量，并因此增加了燃料的消耗。这也增大了压力容器在车辆上占据的空间。
多层类型的衬里一般包括六层的结构：基于热塑性材料(优选地为HDPE)的内层；第一粘合剂层；包括阻隔性树脂(优选地为EVOH)的层；第二粘合剂层；次料(regrind)层；以及基于热塑性材料的外层。为人熟知的是这些已知的衬里遭受氢气在HDPE内层(该HDPE内层与氢气直接接触)中相对高的扩散性的负面影响。氢气可能在HDPE内层内的某些区域集中。该积累在放压时产生气泡。这种气泡形成在此称作“起泡”。该起泡可能会导致损害，该损害的形式为衬里的开裂或机械降解。该结构的另外一个缺点在于它对在加燃料操作期间发生的高度温度变化的耐受性低。通常，衬里暴露于数分钟内从-40℃至+80℃的快速温度变化。这在衬里材料中产生大量热应力，这可能导致衬里断裂。
WO2013108102公开了一种包括修圆容器的压力容器，该修圆容器包括热塑性组合物。该热塑性组合物包括硅氧烷共聚物。该热塑性组合物还包括聚酰胺混合物。然而，该文献不涉及提供具有氢气渗透性低和耐起泡性良好的衬里的容器。而且，WO2013108102不涉及包裹有增强结构的衬里。
在US2009/0203845和DE20201007414中描述了其它压力容器。
鉴于上述缺点，存在对于改进的用于存储氢气的压力容器的需求。
发明内容
因此，本发明的一个方面在于提供一种包括单层衬里的复合材料压力容器，该衬里通过注射模制制成，该衬里包括至少两个可焊接在一起的壳体。有利地，每个壳体由聚合物组合物制成，该聚合物组合物包括相对于所述聚合物组合物的总重量的重量比至少为45％的芳香族聚酰胺和相对于所述聚合物组合物的总重量的重量比至少为10％的脂肪族聚酰胺。
由此，提出一种由聚合物混合物(即聚合物组合物)制成的单层衬里，该聚合物混合物包括相对于聚合物组合物的总重量的重量比至少为45％的芳香族聚酰胺和重量比至少为10％的脂肪族聚酰胺。与已知的基于聚酰胺的单层衬里(即纯PA-6衬里)相比，本发明的聚合物混合物提供的单层衬里在保持低氢气渗透性的同时厚度减小。而且，它提供的单层衬里具有良好的机械强度，以支持例如线缠绕工艺而在线缠绕工艺之后不危害该结构衬里的完好性。
要指出的是，本发明的聚合物混合物的化学特性允许减慢氢气在单层衬里内的迁移(即降低扩散率)。本发明的聚合物混合物提供扩散延迟功能。使用这样的扩散延迟功能允许保护单层衬里免受起泡造成的开裂效应。
本发明的复合材料压力容器能够存储压强高于700bars的气体。
术语“聚合物组合物”指的是具有一种或更多种单体的聚合材料，包括均聚物、共聚物、三元共聚物等。
术语“聚合物组合物”还指两种或更多种聚合物的混合物，并且与术语“聚合物混合物”可换用。本发明的另一方面在于提供一种包括如上所述的复合材料压力容器的车辆。
附图说明
图1示意性地示出根据本发明一个具体实施方式的复合材料压力容器和用于制造这样的复合材料压力容器的方法。
具体实施方式
如图1所示，通过注射模制(或通过注射-压缩模制)分别地制造两个壳体1和2。由于注射模制工艺是常规的，在本领域中为人熟知，将不对其做更详细的说明。这样的注射模制工艺例如在文献US20140312043中有描述。
每个壳体1和2由聚合物组合物制成，该聚合物组合物包括相对于聚合物组合物的总重量的重量比至少为45％的芳香族聚酰胺和相对于聚合物组合物的总重量的重量比至少为10％的脂肪族聚酰胺。例如，本发明的聚合物组合物通过在双螺杆挤出机中干混合芳香族聚酰胺和脂肪族聚酰胺来制备。例如，可在Latech LTE 26-44型双螺杆挤出机中干混合芳香族聚酰胺和脂肪族聚酰胺。
然后将两个壳体1和2焊接在一起以形成单层衬里3。衬里3包括圆柱形部分3a和在圆柱形部分的两端处形成的两个圆拱形部分3b、3c。每个圆拱形部分3b、3c的顶部可附接有金属口部3d、3e。使用注射模制工艺是一个优点，这是因为衬里显示出良好的尺寸准确性，并且衬里与金属口部之间的界面随着时间推移并在耐久性测试期间保持密封。可通过以下方式获得衬里与金属口部之间更高的密封：
-非常精确地压缩在衬里与金属口部之间的密封件；
-对衬里和金属口部的良好的表面处理；
-对衬里和金属口部的厚度的良好控制。
例如，在衬里3上布置有线缠绕4。线缠绕(碳或玻璃的纤维)形成增强结构。可使用其它增强结构。例如，可使用TW(Tape Winding，即带缠绕)方法。TW方法是其中围绕着衬里缠绕带状预浸材料的方法。替代地，可使用“编辫”方法以通过编织数条纤维束在衬里外围上形成主体，该主体浸渍有待熟化的树脂。
本发明的聚合物组合物包括相对于聚合物组合物的总重量的重量比至少为45％的芳香族聚酰胺和重量比至少为10％的脂肪族聚酰胺。
在本发明中，芳香族聚酰胺是在聚合物链中包括至少一个“1型”重复单元的聚合物，该重复单元具有至少一个CONH基团和至少一个芳香族基团。尽管不是必须的，这样的芳香族基团一般源自二元酸单体，包括对苯二甲酸(TA)、间苯二甲酸(IPA)、邻苯二甲酸、十二烷二酸等。芳香族残基的特征在于存在通常具有6个碳原子的芳香环。
在一个优选实施方式中，芳香族聚酰胺在聚合物链中的重复结构单元中包含至少30％摩尔比的芳香族残基。
对于本发明有用的芳香族聚酰胺的非限制性例子包括：聚芳基酰胺MXD6(由Solvay销售的IXEF级)或聚邻苯二甲酰胺(Solvay的
Figure BDA0002017803550000051
级、或Dupont的
Figure BDA0002017803550000052
或EMS的
Figure BDA0002017803550000053
HT)。
在本发明中，脂肪族聚酰胺是在聚合物链中包括至少一个“2型”重复单元的聚合物，该重复单元具有至少一个CONH基团。而且，2型重复单元的特征在于其中包括0％摩尔比的芳香族基团。由此，在脂肪族聚酰胺中包含芳香族基团的重复单元的最大含量在此是基于聚合物中100％摩尔比的重复单元的0％摩尔比。尽管不是必须的，这样的脂肪族基团可源自二元胺单体，包括具有4至12个碳原子的脂肪族二元胺，例如六亚甲基二胺(HMDA)、壬二胺、2-甲基-1,5-戊二胺和1,4-丁二胺等。脂肪族单元的一个有用的二元酸来源是己二酸。在本发明中有用的脂肪族聚酰胺是脂肪族尼龙(例如：PA6、PA6.6、PA6.12、PA4.6、PA11、PA12等)。
本发明的聚合物组合物具有例如氢气渗透性、机械特性和焊接性能等特性的良好平衡。
如将在下文所述(见表1)，本发明的聚合物组合物具有比纯PA6组合物更低的氢气渗透性。它还具有良好的耐起泡性，并能够耐受加燃料操作期间的高度温度变化，其特征在于介于280℃至305℃之间的熔融温度范围。
如果芳香族聚酰胺相对于聚合物组合物的总重量低于45％，则聚合物组合物将具有不令人满意的机械特性。
如果脂肪族聚酰胺相对于聚合物组合物的总重量的重量比低于10％，则聚合物组合物将具有不令人满意的焊接性能。
优选地，芳香族聚酰胺与脂肪族聚酰胺的重量比介于1.4至9之间，脂肪族聚酰胺相对于聚合物组合物的总重量的含量大于或等于10％并小于35％重量比，并且芳香族聚酰胺相对于聚合物组合物的总重量的含量大于或等于45％重量比。
在一个具体实施方式中，本发明的聚合物组合物包括65％至90％重量比的芳香族聚酰胺(通过如PCT/EP2017/069070中所述的NMR光谱来测量)，和10％至35％重量比的脂肪族聚酰胺(通过如PCT/EP2017/069070中所述的NMR光谱来测量)。
如果芳香族聚酰胺相对于聚合物组合物的总重量的重量比在90％以上，则聚合物组合物具有较低的焊接性能(即通过焊接两个半壳体获得的储箱的爆裂压力低于4bars)。
如果芳香族聚酰胺相对于聚合物组合物的总重量的重量比在65％以上，则聚合物组合物具有改进的根据ISO527以1毫米/分钟在60℃下的拉伸模量。当芳香族聚酰胺相对于聚合物组合物的总重量的重量比为65％时，所获得的拉伸模量高于500MPa。衬里在老化期间的变形由此被减小。
这些比例是通过NMR光谱、更具体地说通过13C NMR光谱(如PCT/EP2017/069070中所述)来测量的。
一类优选的芳香族聚酰胺是聚邻苯二甲酰胺(PPA)。根据ASTM D5336标准，PPA是如下芳香族聚酰胺：其中，对苯二甲酸或间苯二甲酸的残基或这两者的组合占聚合物链中的重复结构单元的二羧酸部分的至少55％摩尔比。PPA包含超过55％摩尔比的通过至少一种邻苯二甲酸与至少一种脂肪族二元胺之间的缩聚反应形成的重复结构单元。该脂肪族二元胺尤其可以是六亚甲基二胺、三甲基六亚甲基二胺、壬二胺、2-甲基-1,5-戊二胺和1,4-丁二胺、脂环族二胺。
聚邻苯二甲酰胺包括例如PA6T、PA6T/6I或PA6T/6I/66，以及它们的混合物。
这样的组合物在市场上有销售。
在一个具体实施方式中，所述芳香族聚酰胺是聚邻苯二甲酰胺。
其它可用的芳香族聚酰胺类是聚芳基酰胺或PMXDAs，即包括超过50％摩尔比的通过至少一种脂肪族二元酸(例如己二酸)和间苯二甲胺之间的缩聚反应形成的循环单元的这样的芳香族聚酰胺。基于间苯二甲胺的芳香族聚酰胺的一个实施例是PA MXD 6。
以下参照表1更详细地说明本发明的聚合物组合物的优点。
在Latech LTE 26-44型双螺杆挤出机中干混合67％的芳香族聚酰胺(例如在市场上有销售的
Figure BDA0002017803550000071
AT1001L)和33％的脂肪族聚酰胺(例如在市场上有销售的PA6
Figure BDA0002017803550000072
C548B)，以制备目标聚合物组合物颗粒。所获得的颗粒被注射模制以生产厚度为3mm的10x10cm2的试样。
为了测量氢气，使用气体吹扫法(purge gas method)。测试是根据ASTM D-3985和DIN 53380-3标准进行的。
测试是在23℃下进行的。在测试期间温度恒定。
用电化学传感器检测氢气。
特别地，使用氢气泄露检测器来量化氢气泄露情况。检测极限是0.1ppm(即痕量浓度)。
试样被放置在测量单元中并被夹住。试样暴露于氢气渗透的表面是直径为60mm的盘(2.83*10-3m2)。
通过加压(绝对压强为10bar±1bar)气瓶在0％相对湿度和以99.999％的高纯度氢气来供给氢气。
在渗透侧，通过质量流量控制器或蠕动泵供给合成空气(0％相对湿度)。该合成空气用作吹扫气体。流率是15至70ml min-1。
试样的厚度为3mm，但可使用其它厚度。
这样的测试可例如通过德国Mecadi公司的网站www.mecadi.com上Chemicals/Processing页面介绍的方法来进行。
评估了试样的氢气可渗透性。所获得的结果在表1中示出。
表1
Figure BDA0002017803550000081
本发明的聚合物组合物的较低渗透性允许将总厚度从通常的4mm(在注射模制的纯PA6衬里上)减小到3mm。衬里厚度的最终减小通常允许针对车辆上的给定空间增加1L的氢气存储，并使得复合材料压力容器的重量减小至少1kg。

Claims (7)

1.一种复合材料压力容器，包括单层衬里和布置在所述衬里上的增强结构，所述衬里通过注射模制制成，所述衬里包括至少两个可焊接在一起的壳体，其中每个壳体由聚合物组合物制成，所述聚合物组合物包括相对于所述聚合物组合物的总重量的重量比至少为45％的芳香族聚酰胺和相对于所述聚合物组合物的总重量的重量比至少为10％的脂肪族聚酰胺，在脂肪族聚酰胺中包含芳香族基团的重复单元的最大含量是基于该聚合物中100％摩尔比的重复单元的0％摩尔比，其中所述芳香族聚酰胺是聚邻苯二甲酰胺(PPA)。
2.如权利要求1所述的复合材料压力容器，其中，所述聚合物组合物包括相对于所述聚合物组合物的总重量的重量比为65％至90％的芳香族聚酰胺和相对于所述聚合物组合物的总重量的重量比为10％至35％的脂肪族聚酰胺。
3.如权利要求1或2所述的复合材料压力容器，其中，所述芳香族聚酰胺选自PA6T、PT6T/6I和/或PA6T/6I/66及其混合物。
4.如权利要求1至2中任一项所述的复合材料压力容器，其中，所述脂肪族聚酰胺选自PA6、PA6.6、PA6.12、PA4.6、PA11和/或PA12。
5.如权利要求4所述的复合材料压力容器，其中，所述脂肪族聚酰胺是PA6或/和PA6.6。
6.如权利要求1至2中任一项所述的复合材料压力容器，其中，所述增强结构是线缠绕或带缠绕。
7.一种车辆，该车辆包括如权利要求1至6中任一项所述的复合材料压力容器。
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