CN111566153A - 用于航空内饰的pei颗粒泡沫 - Google Patents
用于航空内饰的pei颗粒泡沫 Download PDFInfo
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- CN111566153A CN111566153A CN201880067073.9A CN201880067073A CN111566153A CN 111566153 A CN111566153 A CN 111566153A CN 201880067073 A CN201880067073 A CN 201880067073A CN 111566153 A CN111566153 A CN 111566153A
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Abstract
基于聚醚酰亚胺(PEI)的聚合物泡沫满足航空工业对航空内饰要求的法律规范。特别是,对防火特性、耐介质性和机械性质的要求在此构成巨大的挑战。根据现有技术,作为半成品形式生产合适的聚合物泡沫。例如由于大量的切削废料,再加工成模制品在时间和材料利用方面不经济。本发明通过可将原则上合适的材料加工成颗粒泡沫模制品而解决这一问题。这些模制品可在短周期时间内生产而无需再加工,并因此经济地生产。此外,这带来新的功能集成的可能性,例如通过在泡沫中直接引入嵌件等,和在设计自由度方面。
Description
技术领域
基于聚醚酰亚胺(PEI)的聚合物泡沫满足航空工业对航空内饰要求的法律规范。特别是,对防火特性、耐介质性和机械性质的要求在此构成巨大的挑战。根据现有技术,作为半成品形式生产合适的聚合物泡沫。例如由于大量的切削废料,再加工成模制品在时间和材料利用方面不经济。本发明通过可将原则上合适的材料加工成颗粒泡沫模制品而解决这一问题。这些模制品可在短周期时间内生产而无需再加工,并因此经济地生产。此外,这带来新的功能集成的可能性,例如通过在泡沫中直接引入嵌件等,和在设计自由度方面。
背景技术
适用于航空工业中安装的泡沫材料是公知的。但是,为此用途描述的大多数泡沫只是由纯PMI(聚甲基丙烯酰亚胺)、PPSU(聚苯砜)或PES(聚醚砜)构成的泡沫。在文献中也发现了PI(Polyarylimid),尽管其从毒理学的角度看不合适。所有这些材料迄今仅作为块状或板状材料使用。
也有其它材料不太详细地被描述作为板状材料用于航空工业中安装。例如,聚(氧基-1,4-苯基磺酰基-1,4-苯基)(PESU)是这种材料。这例如由DIAB公司以Divinycell F产品名出售。但是,在这些挤出泡沫板的进一步加工中,产生不经济的大量边角料。
在三维泡沫模制品的生产中避免切削废料的经济的方法是使用泡沫颗粒(珠粒泡沫)代替块状泡沫。根据现有技术可得的所有颗粒泡沫在高温下使用的情况下具有缺点,或总体上,尤其是在这些高温下,具有非最佳的机械性质。此外,已知只有很少数的泡沫不易燃并因此可例如安装在公路、轨道或空中交通工具的内部。例如,基于聚丙烯(PP)、聚苯乙烯(EPS)、热塑性聚氨酯弹性体(E-TPU)或PMI(ROHACELLTriple F)的颗粒泡沫具有不足的阻燃性,而原则上合适的所有固有阻燃的聚合物,例如PES、PEI或PPSU根据现有技术仅加工成块状泡沫。
发明内容
问题
考虑到现有技术,本发明要解决的问题在于提供一种用于生产用于航空器构造的新型泡沫或复合材料的组合物,所述复合材料可以是例如具有热塑性或交联覆盖层的泡沫芯。在此,所得泡沫应具有在高温下的可用性、良好机械性质,尤其是足够的断裂伸长率,和对汽车和航空器构造领域中的许多用途而言至少足够的阻燃性的良好结合。
更特别地,该泡沫在此应具有对各种液体(酸性、碱性或疏水液体)和对乳液的高耐受性。
此外,该泡沫应该可由待开发的组合物通过各种不同的方法和以多种多样的三维形状实现,并且在最终组件的生产中产生尽可能少的或者仅非常少的边角料。
其它非明示的问题可能从本文中的说明书、权利要求书或实施例中显而易见,而在此不为此明确列举。
解决方案
通过提供用于生产航空工业中,尤其是航空器构造中所用的不易燃的热稳定泡沫材料的新型组合物解决了这些问题。用于生产泡沫的这种本发明的组合物的特征在于,其是基于聚醚酰亚胺(PEI)的颗粒泡沫。根据本发明的颗粒泡沫在此作为已发泡材料具有180至215℃的玻璃化转变温度,并且其中颗粒泡沫的平均泡孔直径小于2mm,优选小于1mm,更优选小于500μm,最优选小于250μm。
这尤其是令人惊讶的,因为PEI的实际玻璃化转变温度为215至217℃,因此该材料根据现有技术,例如借助水下制粒,无法加工成颗粒泡沫。
根据本发明,术语“泡孔”描述泡沫中的不含任何基体材料但至少部分被其包围的区域。泡孔在此也被称为孔隙。理想地,在硬质泡沫中,这些孔隙或泡孔是封闭的,这又意味着泡孔完全被泡沫的基体材料包围。在较软质泡沫的情况下,至少部分地存在开放的泡孔。这些可通过不完整壁的排列或在桥接结构的极端情况下仍被识别为独立泡孔。因此也有可能测定此类开孔的尺寸。在许多情况下可以简单的方式,例如借助显微镜,测量泡孔的尺寸。也在考虑这些因素的情况下,保持泡沫中的最大泡孔尺寸对于本领域技术人员而言是简单的。
泡沫颗粒根据本发明被理解为是指通过单个未发泡或预发泡颗粒的发泡界定的颗粒泡沫中的区域。互相结合的单个泡沫颗粒之间的边界可以是肉眼易见的或可在光学显微镜下测定。当两个泡沫颗粒之间的界面显而易见时,这尤其适用。但是,由于情况不定必定如此,本发明使用简化方法:为此,以简单方式由未发泡颗粒的直径、未发泡颗粒的总体积和成品泡沫件的体积计算泡沫颗粒的理论平均直径。本领域技术人员知道,在颗粒泡沫的情况下,可以仅在泡沫件的边缘区域中发生小偏差的方式实现泡沫颗粒的规则尺寸分布。本发明的另一个优点在于,单个泡沫颗粒之间的围绕间隙的体积比例如此小,以致其几乎不体现在成品泡沫件的体积测量中。优选地,成品泡沫中的这些泡沫颗粒小于1cm,更优选小于0.7cm。
根据本发明,除非另有说明,报道的玻璃化转变温度借助DSC(差示扫描量热法)测量。在这方面,本领域技术人员知道,只有在第一加热周期直至比最高玻璃化转变或熔融温度高最少25℃、但在此比材料的最低分解温度低至少20℃的温度后,将材料样品在此温度下保持至少2分钟时,DSC才足够有说服力。此后,将样品再次冷却回比要测定的最低玻璃化转变或熔融温度低至少20℃的温度,其中冷却速率应该不高于20℃/min,优选不高于10℃/min。在进一步等待几分钟的时间后,进行实际测量,其中样品以通常10℃/min或更低的加热速率加热到最高熔融或玻璃化转变温度以上至少20℃。
优选地,在本发明的第一个备选实施方案中,用于生产颗粒泡沫的本发明的组合物由80重量%至99.5重量%的PEI组成。此外,这种组合物包括0.5重量%至10重量%,优选1重量%至9重量%的发泡剂。其可进一步尤其含有0重量%至10重量%,优选1重量%至5重量%的添加剂。
添加剂尤其可以是阻燃剂、增塑剂、颜料、紫外线稳定剂、成核剂、抗冲改性剂、粘附性促进剂、流变改性剂、扩链剂、纤维和/或纳米粒子。
所用阻燃剂通常是磷化合物,特别是磷酸盐、膦或亚磷酸盐。合适的紫外线稳定剂和/或紫外线吸收剂是本领域技术人员公知的。HALS化合物、Tiuvine或三唑常用于此用途。所用抗冲改性剂通常是包含弹性体和/或柔性相的聚合物颗粒。它们经常是具有外壳的核-(壳-)壳颗粒,所述外壳本身最多轻度交联并作为纯聚合物表现出与PEI的至少最低限度的混容性。作为颜料,原则上可使用任何已知的颜料。特别对于较大的量,当然要测试它们对发泡操作的影响,就像所有其它以多于0.1重量%的较大量使用的添加剂的情况下那样。这对本领域技术人员而言可采用较小的成本和复杂程度实施。
合适的增塑剂、流变改性剂和扩链剂是由PEI或含PEI的共混物生产箔、膜或模制品的领域中的本领域技术人员公知的,并因此可以低成本和复杂程度转用到由根据本发明的组合物生产泡沫。
任选添加的纤维通常是已知的可添加到聚合物组合物中的纤维材料。在本发明的一个特别合适的实施方案中,该纤维是PEI纤维、PES纤维、PPSU纤维或共混纤维,后者选自所提到的聚合物。
纳米粒子,可例如以管、薄片、杆、球体的形式或以其它已知形式存在,通常是无机材料。它们可在最终泡沫中同时发挥各种功能。例如,这些粒子部分情况下充当发泡操作中的成核剂。所述粒子可另外影响泡沫的机械性质,以及(气体)扩散性质。所述粒子另外对难燃性额外作出贡献。
除所列举的纳米粒子外,也可添加微米粒子或较不混容的相分离聚合物作为成核剂。就组成而言,所述聚合物在此必须与其它成核剂分开考虑,因为后者主要影响泡沫的机械性质、该组合物的熔体粘度和因此影响发泡条件。相分离聚合物作为成核剂的额外作用是这种组分的额外希望的作用,但在这种情况下不是主要作用。因此,这些附加聚合物进一步与其余添加剂分开列举在总体合计。
添加剂中任选也有可能包括最多9重量%的附加聚合物组分以调节物理性质。附加聚合物可以例如是聚酰胺、聚烯烃,特别是PP,聚酯,特别是PET,硫基聚合物,例如PSU、PPSU、PES或聚(甲基)丙烯酰亚胺。
发泡剂的选择相对自由并且对本领域技术人员而言特别取决于所选发泡方法、在聚合物中的溶解度和发泡温度。合适的实例是醇,例如异丙醇或丁醇,酮,如丙酮或甲乙酮,烷烃,如异丁烷或正丁烷,或异戊烷或正戊烷,己烷、庚烷或辛烷,烯烃,例如戊烯、己烯、庚烯或辛烯,CO2、N2、水、醚,例如二乙醚,醛,例如甲醛或丙醛,氟(氯)烃、化学发泡剂或这些物质中两种或更多种的混合物。
化学发泡剂是较不挥发或完全不挥发的物质,其在发泡条件下发生化学分解并在此形成实际发泡剂。叔丁醇是用于此的一个非常简单的实例,其在发泡条件下形成异丁烯和水。进一步的实例是NaHCO3、柠檬酸、柠檬酸衍生物、偶氮二甲酰胺(ADC)和/或基于其的化合物、甲苯磺酰肼(TSH)、氧代双(苯并磺酰肼)(OBSH)或5-苯基四唑(5-PT)。
优选地,根据本发明的颗粒泡沫具有大于0.5MPa的根据ISO1926的拉伸强度、8%至12%的根据ISO1926的断裂伸长率、大于8MPa的根据ASTM C273在室温下的剪切模量、大于0.45MPa的根据ASTMC273在室温下的抗剪切强度、大于13MPa的根据ISO 844在室温下的压缩模量和大于0.4MPa的根据ISO 844在室温下的压缩强度。在使用下文描述的方法生产颗粒泡沫的情况下,在保持根据本发明的玻璃化转变温度和泡孔尺寸的同时保持这些机械性质对本领域技术人员而言是简单的事情。此外,还已经发现,令人惊讶地,根据本发明的颗粒泡沫可在满足根据FAR 25.852的防火规范或防火性质下使用,所述防火规范或防火性质对于在航空工业中,特别是用于航空器内部是重要的。
也非常令人惊讶的是,根据本发明的颗粒泡沫,就像相应的板状泡沫那样,满足用于航空器内部所必需的所有材料性质。对于例如PMI而言,不存在这种关联,因为由块状泡沫得到的这种聚甲基丙烯酰亚胺片材满足这些条件,而颗粒泡沫经常具有比块状泡沫差的机械性质。已另外发现的特别令人惊讶的优点在于,这种颗粒泡沫,不同于块状泡沫,没有明显的直至根本没有泡孔取向。这在许多情况下赋予颗粒泡沫有利的各向同性的机械性质,而相应的块状泡沫经常具有各向异性的机械性质,使得它们在一个区域中和在与这一区域垂直的轴中不同。根据具体用途,各向同性机械性质可能是相当有利的,尤其是当来自各个不同方向的压力应力均等时。
优选地,根据本发明的泡沫的发泡度相当于1%至98%,优选50%至97%,更优选70%至95%的相对于未发泡材料的密度降低。该泡沫优选具有20至1000kg/m3,优选40至250kg/m3,尤其优选50至150kg/m3的密度。
除根据本发明的颗粒泡沫外,其生产方法也是本发明的组成部分。
原则上,有两种优选方法用于生产根据本发明的PEI颗粒泡沫。在第一种方法变体中,借助具有孔板的挤出机加工由80重量%至99.5重量%的PEI、0.5重量%至10重量%的发泡剂和0重量%至10重量%的添加剂组成的组合物,以产生发泡或可发泡粒料。在此,进料区与螺杆尖端之间的温度优选在320至400℃的范围内。此外,在这一段路径上通常不存在均一温度,而是存在例如具有沿聚合物熔体的传送方向温度递增的梯度。孔板的温度在此在250至350℃之间,并且经孔板离开时的物料温度在230至360℃之间。通常在此在挤出机中加载发泡剂。粒料然后在水下制粒中的压力低于发泡剂的膨胀力时在其离开孔板时发泡。由此发泡的粒料随后优选进一步加工成颗粒泡沫。
在这一实施方案的一个变体中,可将离开挤出机的组合物导入水下制粒机。这种水下制粒机在此被设计为具有防止发泡的温度和压力的组合。这种程序获得加载有发泡剂的粒料,其可稍后通过重新供应能量发泡到所需密度和/或通过任选成型进一步加工成颗粒泡沫工件。可以借助例如在空气循环炉中的接触加热或借助红外或微波辐射而以基于辐射的方式实现预发泡所需的能量输入。
在用于生产PEI颗粒泡沫的第二种方法变体中,首先同样借助具有孔板的挤出机加工由90重量%至100重量%的PEI和0重量%至10重量%的添加剂组成的组合物以产生粒料,但在此没有加载发泡剂。在进料区与螺杆尖端之间的温度在此也在320至400℃的范围内,其再次不必定是均匀的。孔板的温度同样在250至350℃之间,并且经孔板离开时的物料温度在230至360℃之间。在此,该粒料随后在高压釜中加载发泡剂以使得它们然后含有0.5重量%至10重量%的发泡剂。加载有发泡剂的粒料可随后通过泄压和/或通过加热到超过200℃的温度而发泡以获得颗粒泡沫。
就实际发泡而言,原则上各种使聚合物组合物发泡的方法是本领域技术人员已知的,其特别是在用于热塑性泡沫的方法方面适用于本发明组合物。例如,该组合物可在150至250℃的温度和0.1至2巴的压力下发泡。优选地,实际发泡,如果没有接在挤出后,其在标准压力气氛中在180至230℃的温度下实施。
在稍后加载发泡剂的变体中,仍无发泡剂的组合物在高压釜中在例如20至120℃的温度和例如30至100巴的压力下与发泡剂混合,并随后在高压釜内通过降低压力和提高温度到发泡温度而发泡。或者,与发泡剂混合的组合物在高压釜中冷却并在冷却后取出。这种组合物可稍后通过加热到发泡温度而随后发泡。这也可例如在进一步成型下或与其它元件如嵌件或覆盖层组合进行。
特别优选地,制成的颗粒泡沫–无论所用方法如何–随后与覆盖材料胶粘、缝合或焊接。“焊接”在此是指组件的加热导致材料之间的内聚或粘合,例如通过泡沫表面的开孔被覆盖材料部分填充。
覆盖材料可以是木材、金属、装饰箔、复合材料、预浸料坯或其它已知材料。
在所用材料稍后发泡的情况下,例如在高压釜中加载发泡剂之后,制成的颗粒泡沫也可另选在覆盖材料存在下发泡,以使得覆盖材料与颗粒泡沫借助胶粘或焊接结合。
在挤出机中加载发泡剂的方法变体中,PEI也可另选在离开挤出机时加到任选加热的、任选含有覆盖材料的模具中。在这种情况下,在成型的同时实现发泡以产生颗粒泡沫或复合材料。或者,可将离开挤出机的组合物导入泡沫喷涂装置。在这种装置中,随后直接在成型的同时发泡。
无论所用变体如何,可在发泡过程中为颗粒泡沫或复合材料提供嵌件和/或可将通道引入颗粒泡沫中。
根据本发明的泡沫或通过根据本发明的方法制成的泡沫可用于航天器或航空器的构造,尤其是在其内部或外部。这在此可包括颗粒泡沫,无论是否通过本发明的方法制成,同样还可包括由此实现的复合材料。更特别地,由于它们的难燃性,本发明的泡沫也可安装在这些交通工具的内部。
更特别地,纯PEI颗粒泡沫尤其适合引入航空器内部。航空器在此除包括喷气式飞机或小型飞机外,尤其还包括直升飞机或甚至航天器。安装在这样的航空器内部的实例是,例如,可在客机座椅背面向下折叠的小桌板、座椅填充物或内部隔断,以及例如内门。
基于含PEI的共混物的颗粒泡沫另外也适合还引入航空器外部。“外部”在此不仅是指作为航空器外壳中的填充物,还尤其也在机头、尾区、机翼、外门、操纵面或转子叶片中。
Claims (13)
1.PEI颗粒泡沫在航空器构造中的用途,其特征在于所述发泡PEI具有180至215℃的玻璃化转变温度,并且所述颗粒泡沫的平均泡孔直径小于2mm。
2.根据权利要求1的颗粒泡沫的用途,其特征在于所述颗粒泡沫从由80重量%至99.5重量%PEI、0.5重量%至10重量%的发泡剂和0重量%至10重量%的添加剂组成的组合物获得。
3.根据权利要求1或2的颗粒泡沫的用途,其特征在于所述添加剂是阻燃剂、增塑剂、颜料、紫外线稳定剂、成核剂、抗冲改性剂、粘附性促进剂、流变改性剂、扩链剂、纤维和/或纳米粒子。
4.根据权利要求1至3中至少一项的颗粒泡沫的用途,其特征在于所述发泡剂是醇、酮、烷烃、烯烃、CO2、N2、水、醚、醛、化学发泡剂或这些物质中两种或更多种的混合物。
5.根据权利要求1至4中至少一项的颗粒泡沫的用途,其特征在于所述颗粒泡沫具有大于0.5MPa的根据ISO1926的拉伸强度、8%至12%的根据ISO1926的断裂伸长率、大于8MPa的根据ASTM C273在室温下的剪切模量、大于0.45MPa的根据ASTM C273在室温下的抗剪切强度、大于13MPa的根据ISO 844在室温下的压缩模量和大于0.4MPa的根据ISO 844在室温下的压缩强度。
6.根据权利要求1至5中至少一项的颗粒泡沫的用途,其特征在于所述颗粒泡沫安装在航空器内部。
7.根据权利要求1至6中至少一项的颗粒泡沫的用途,其特征在于所述颗粒泡沫的平均泡孔直径小于500μm。
8.生产用于根据权利要求1至7中至少一项的用途的PEI颗粒泡沫的方法,其特征在于借助具有孔板的挤出机,加工由80重量%至99.5重量%的PEI、0.5重量%至10重量%的发泡剂和0重量%至10重量%的添加剂组成的组合物,以产生发泡粒料,其中进料区与螺杆尖端之间的温度在180至380℃的范围内,孔板的温度在250至350℃之间,并且经孔板离开时的物料温度在230至360℃之间,并且发泡粒料随后进一步发泡成颗粒泡沫。
9.生产用于根据权利要求1至7中至少一项的用途的PEI颗粒泡沫的方法,其特征在于借助具有孔板的挤出机,加工由90重量%至100重量%的PEI和0重量%至10重量%的添加剂组成的组合物,以产生粒料,其中进料区与螺杆尖端之间的温度在180至380℃的范围内,孔板的温度在300至350℃之间,并且经孔板离开时的物料温度在250至360℃之间,并且所述粒料随后在高压釜中加载发泡剂,以使得它们因此含有0.5重量%至10重量%的发泡剂,并且加载有发泡剂的粒料随后通过膨胀和/或通过加热到超过200℃的温度发泡以获得颗粒泡沫。
10.生产复合部件的方法,其特征在于将借助根据权利要求8或9的方法制成的颗粒泡沫与覆盖材料胶粘、缝合或焊接。
11.生产复合部件的方法,其特征在于借助根据权利要求8或9的方法制成的颗粒泡沫在覆盖材料存在下发泡,以使得所述覆盖材料借助胶粘或焊接与颗粒泡沫结合。
12.根据权利要求8的方法,其特征在于所述PEI在离开挤出机后引入任选加热的、任选含有覆盖材料的模具中,并在此在成型的同时发泡以产生颗粒泡沫或复合材料。
13.根据权利要求8至12中至少一项的方法,其特征在于在发泡过程中将嵌件和/或通道引入颗粒泡沫中。
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PCT/EP2018/072392 WO2019038213A1 (de) | 2017-08-24 | 2018-08-20 | Pei-partikelschäume für anwendungen im luftfahrt-interieur |
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US20230105032A1 (en) | 2023-04-06 |
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MX2020001993A (es) | 2020-09-25 |
US11814499B2 (en) | 2023-11-14 |
BR112020003712A2 (pt) | 2020-09-01 |
RU2020111351A3 (zh) | 2021-09-28 |
US20200207939A1 (en) | 2020-07-02 |
TW201920405A (zh) | 2019-06-01 |
JP7315534B2 (ja) | 2023-07-26 |
ZA202001702B (en) | 2021-05-26 |
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WO2019038213A1 (de) | 2019-02-28 |
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