CN111406091A - 用于在航空器内部中应用的pesu粒子泡沫 - Google Patents

用于在航空器内部中应用的pesu粒子泡沫 Download PDF

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Publication number
CN111406091A
CN111406091A CN201880076517.5A CN201880076517A CN111406091A CN 111406091 A CN111406091 A CN 111406091A CN 201880076517 A CN201880076517 A CN 201880076517A CN 111406091 A CN111406091 A CN 111406091A
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CN
China
Prior art keywords
pesu
particle foam
foam
temperature
foamed
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Pending
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CN201880076517.5A
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English (en)
Inventor
C·特拉斯尔
D·霍林
K·伯恩哈德
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Evonik Operations GmbH
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Evonik Operations GmbH
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Publication of CN111406091A publication Critical patent/CN111406091A/zh
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Abstract

基于聚醚砜(PESU)的聚合物泡沫满足由航空工业对于航空器内部所要求的法律规范。尤其是对燃烧特性、介质稳定性和机械性能的要求在此构成了巨大的挑战。根据现有技术，合适的聚合物泡沫是作为半成品制备的。就时间和材料利用而言，再加工以获得模制品是不经济的，例如由于大量的切割废料。本发明通过如下方式解决了这个问题：可将原则上适合的材料加工以获得粒子泡沫模制品。这些模制品可在短周期时间内制备而无需再加工，并且因此被经济地制备。另外，这得到了新的功能整合的可能性，例如通过在所述泡沫中直接引入插件等，以及关于在设计方面的自由度的可能性。

Description

用于在航空器内部中应用的PESU粒子泡沫
技术领域
基于聚醚砜(PESU)的聚合物泡沫满足由航空工业对于航空器内部所要求的法律规范。尤其是对燃烧特性、介质稳定性和机械性能的要求在此构成了巨大的挑战。根据现有技术，合适的聚合物泡沫是作为半成品制备的。就时间和材料利用而言，再加工以获得模制品是不经济的，例如由于大量的切割废料。本发明通过如下方式解决了这个问题：可将原则上适合的材料加工以获得粒子泡沫模制品。这些模制品可在短周期时间内制备而无需再加工，并且因此被经济地制备。另外，这得到了新的功能整合的可能性，例如通过在所述泡沫中直接引入插件等，以及关于在设计方面的自由度的可能性。
背景技术
PES和PPSU的共混物对于其它技术应用完全是已知的。例如，EP 1 497 376描述了用于在熔融成型、注射模塑、压缩模塑、挤出或吹塑中进行加工的相应的共混物。然而，由这种组合物制备泡沫材料是未知的。
在航空工业中已经作为板材料被安装的一种对此的替代材料是聚(氧基-1,4-苯基磺酰基-1,4-苯基)(PESU)。这例如以商品名Divinycell F由DIAB公司销售，或者以Radel商品名由Solvay公司销售。然而，在这些挤出泡沫板的进一步加工中，不经济地产生大量的下脚料。
例如在EP 0 764 461中也描述了由这些共混物制备的多孔膜。这种膜是由水性聚合物组合物借助于浇铸方法制备的。
许多工业上使用的泡沫材料要么在高温下的使用过程中有缺点，要么在整体上，并且特别是在这些高温下，具有非最佳的机械性能。另外，只已知非常少的泡沫材料不是易燃的并且因此可例如安装在公路车辆、轨道车辆或飞机的内部空间中。例如，PES泡沫具有差的阻燃效果，而PPSU泡沫例如具有非最佳的断裂强度。
得自PPSU或PES的泡沫材料原则上是已知的，然而它们没有彼此混合。例如，在L.Sorrentino的“Polymeric Foams from High-Performance Thermoplastics(得自高性能热塑性塑料的聚合物泡沫)”,Advances in Polymer Technology,第30卷,第3期,第234-243页,2011(DOI 10.1002/adv)中报道了用于确认使PPSU和/或PES发泡的理想条件的相应研究。
包含PPSU或PSE的共混物同样是已知的，然而在现有技术中提供的细节相当少。例如，这两种聚合物都已经尤其被描述为例如在PS泡沫中作为用量上次要的组分，以影响这些商品材料的性能。相反，包含PPSU或PES作为主要组分的泡沫仅在非常少的说明中找到，例如在以下文献中：
US 4,940,733公开了基于一种共混物的泡沫材料，所述共混物是聚碳酸酯与第二聚合物的共混物，所述第二聚合物除大量其它实例外还可是PES或PPSU。尽管这种类型的泡沫具有高水平的热稳定性，但其阻燃效果不是特别好。关于机械性能也没有提供任何细节。
WO 2015/097058描述了基于PPSU或PES的泡沫材料，其包含至少10重量％的聚烯烃。该相分离的聚烯烃在此主要起到成核剂的作用。在此，尽管获得了更均匀的孔，但阻燃性能或机械性能(例如断裂伸长率)没有被有利影响。实际上，由于相分离甚至可能预期较差的断裂伸长率。阻燃性也可能由于掺混聚烯烃组分而预期变差。
US 2013/0059933、US 2012/13599528和EP 2 692 519描述了向其中添加了最高至10重量％的另一种聚合物(例如聚丙烯酸酯)的PS粒子泡沫。这些泡沫在具有防火需要的应用中全都是不适合的。在DE 102011110216中，也将少量的聚砜或聚醚砜添加到这样的PS粒子泡沫中。然而，这种泡沫同样主要由PS组成，这对于在航空中的应用带来相应的缺点。
发明内容
要解决的技术问题
鉴于现有技术，本发明要解决的问题是提供一种组合物，其用于制备在飞机构造中使用的新型泡沫材料或复合材料。在此，所得的泡沫材料应具有以下性能的良好结合：在高温下的可用性、良好的机械性能(尤其是关于断裂伸长率)和对于在车辆和飞机构造领域中的许多应用至少足够的阻燃作用。
更特别地，所述泡沫材料在此应具有对多种液体、酸、碱或疏水性液体以及对乳液的高耐受性。
另外，所述泡沫材料应可由待开发的组合物通过大量不同的方法并且以非常多样的三维形状实现，并且在最终构件的制备中应尽可能不产生或只产生非常少的下脚料。
其它未明确说明的要解决的问题可从本文的说明书、权利要求书或实施例中得出，而在此不为了这个目的对其明确叙述。
解决方案
所述问题通过提供一种新型组合物得到解决，所述组合物用于制备热稳定的低可燃性泡沫材料，其用于轻质构造，尤其用于航空工业，用于造船工业，用于汽车工业，或用于轨道车辆构造。用于制备泡沫材料的本发明的组合物的特征在于，它是PESU粒子泡沫，其作为经发泡的PESU具有在180和215℃之间的玻璃化转变温度，和其中所述粒子泡沫的平均(mittler)泡孔直径为小于1000μm，优选小于500μm，更优选小于250μm。在此，泡孔被理解为意思是在粒子泡沫中由单独粒子的发泡限定的区域。这是尤其令人惊奇的，因为所述PESU的实际玻璃化转变温度为225℃。
根据本发明，除非另外说明，所报道的玻璃化转变温度是借助于DSC(差示扫描量热法)测量的。对此方面，本领域技术人员知晓的是，只有在如下条件下DSC才是充分确凿的：在第一次加热循环最高至高于最高玻璃化转变温度或熔融温度最小25℃，但低于材料的最低分解温度至少20℃后，使所述材料样品保持在该温度下至少2分钟。之后，将所述样品再次冷却到比待被测定的最低玻璃化转变温度或熔融温度低至少20℃的温度，其中冷却速率应不超过20℃/分钟，优选不超过10℃/分钟。然后，在另外数分钟的等待时间后，进行实际的测量，其中将所述样品在通常10℃/分钟或更小的加热速率下加热直到比最高熔融温度或玻璃化转变温度高至少20℃。
优选地，用于制备PESU的本发明的组合物由80重量％至99.5重量％的PESU组成。此外，这种组合物包含0.5重量％至10重量％，优选1重量％至9重量％的发泡剂。它可尤其进一步含有0重量％至10重量％，优选1重量％至5重量％的添加剂。
所述添加剂可尤其是阻燃剂、增塑剂、颜料、UV稳定剂、成核剂、抗冲改性剂、粘合促进剂、流变学改性剂、扩链剂、纤维和/或纳米粒子。
使用的阻燃剂通常是磷化合物，特别是磷酸酯(盐)、膦或亚磷酸酯(盐)。合适的UV稳定剂和/或UV吸收剂是本领域技术人员公知的。为了这个目的，通常使用HALS化合物、Tiuvine或三唑。使用的抗冲改性剂通常是包含弹性体和/或软相的聚合物粒子。这些聚合物粒子经常是核-(壳-)壳粒子，其具有外壳，所述外壳本身最多轻度交联并且作为纯聚合物会表现出与所述PES和PPSU的共混物具有至少最小的混容性。原则上，任何已知的颜料可用作颜料。当然，尤其在较大量的情况下需要对于对发泡操作的影响进行测试，如所有以高于0.1重量％的较大量使用的其它添加剂的情况中那样。这对于本领域技术人员而言可以较小复杂性和成本实施。
合适的增塑剂、流变学改性剂和扩链剂是本领域技术人员由PES、PPSU或这两者的共混物制备片材、膜或模制品中公知的，并且可相应地在较小成本和复杂性下转用到由根据本发明的组合物制备泡沫上。
所述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，所述纤维是PES纤维、PPSU纤维或共混物纤维，后者得自PSE和PPSU。
纳米粒子，其可例如以小管、小板、棒、球形式或其它已知形式存在，通常是无机材料。它们可以在同一时间在最终的泡沫中发挥多种功能。例如，这些粒子在发泡操作中部分地起到成核剂的作用。所述粒子可进一步影响所述泡沫的机械性能以及(气体)扩散性能。所述粒子还进一步对低可燃性做出额外贡献。
除了列举的纳米粒子外，还可以添加微米粒子或较低混溶性的相分离的聚合物作为成核剂。在此，在考虑组成时，所描述的聚合物必须与其它成核剂分开来看，因为后者主要对所述泡沫的机械性能、对所述组合物的熔体粘度产生影响，并且因此对发泡条件产生影响。相分离的聚合物作为成核剂的额外作用是这种组分的额外希望的效果，但在这种情况下不是主要效果。因此，这些额外聚合物在总计中进一步上文所述与其余添加剂分开考虑。
所述添加剂任选还可以包括最高至9重量％的用于调节物理性能的第二聚合物组分。所述额外聚合物可例如是聚酰胺，聚烯烃，特别是PP，PEEK，聚酯，特别是PET，其它硫基聚合物，例如PSU，聚醚酰亚胺或聚甲基丙烯酰亚胺。
发泡剂的选择是相对自由的，并且对于本领域技术人员而言是特别由选择的发泡方法和发泡温度所确定的。合适的实例是醇，例如异丙醇或丁醇，酮，例如丙酮或甲乙酮，烷烃，例如异丁烷或正丁烷、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，例如乙醚，醛，例如甲醛或丙醛，氟(氯)烃，化学发泡剂或这些物质中的两种或更多种的混合物。
化学发泡剂是较不挥发性或完全非挥发性的物质，其在发泡条件下经历化学分解并在此时形成实际的发泡剂。叔丁醇是它的一个非常简单的实例，因为它在发泡条件下形成异丁烯和水。其它实例是NaHCO3、柠檬酸或柠檬酸衍生物、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(苯磺酰肼)(OBSH)或5-苯基四唑(5-PT)。
优选地，根据本发明的PESU粒子泡沫具有大于0.5MPa的根据ISO1926的抗拉强度，在8％和12％之间的根据ISO1926的断裂伸长率，在室温下大于8MPa的根据ASTM C273的剪切模量，在室温下大于0.45MPa的根据ASTM C273的抗剪切强度，在室温下大于13MPa的根据ISO 844的压缩模量，和在室温下大于0.4MPa的根据ISO 844的压缩强度。在采用进一步下文描述的用于制备所述PESU粒子泡沫的方法的情况下，对于本领域技术人员而言，在保持这些机械性能的同时获得根据本发明的玻璃化转变温度和泡孔尺寸是简单的。此外，还已经发现，令人惊奇地，根据本发明的粒子泡沫在满足航空工业中，尤其是对在飞机内部中使用重要的根据FAR 25.852的防火规范或燃烧性能下可用。
另外非常令人惊奇的是，对于在飞机内部空间的使用是先决条件的所有需要的材料性能都被PESU粒子泡沫所满足，正如它们被以板形式的相应泡沫所满足的那样。例如对于PMI，这种关系不存在，因为对于这种由块状泡沫组成的聚甲基丙烯酰亚胺板材，满足所述条件，而粒子泡沫没有得到认可。
优选地，根据本发明的泡沫材料具有的发泡度使得相对于纯共混物的密度降低在1％和98％之间，优选在50％和97％之间，更优选在70％至95％之间。所述泡沫优选具有在20和1000kg/m3，优选40和250kg/m3之间的密度。
除了所述PESU粒子泡沫外，其制备方法也是本发明的组成部分。
原则上，存在两种用于制备所述PESU粒子泡沫的优选方法。在第一方法变体中，将由80重量％至99.5重量％的PESU，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借助于具有孔板的挤出机加工以形成经发泡的粒料。在此，在进料区和螺杆尖端之间的温度在180和380℃之间的范围内。在这种情况下，通常在这个区段内不存在均一的温度，而是，例如，在聚合物熔体的传送方向上存在具有升高的温度的梯度。所述孔板的温度在此在300和350℃之间，和当穿过所述孔板离开时，物料温度在200和360℃之间。在此通常是在挤出机中进行加载所述发泡剂。所述粒料然后当它们从所述孔板离开时发泡。因此发泡的粒料然后优选被进一步发泡以获得粒子泡沫。
在这个实施方案的一个变体中，所述组合物当从所述挤出机中离开时可被引导到水下造粒机中。这种水下造粒机在此在温度和压力的组合方面被设计为使得发泡被阻止。这个过程提供了加载有发泡剂的粒料，其可然后通过重新供应能量发泡到希望的密度和/或通过任选的成型进一步加工成粒子泡沫工件。
在用于制备PESU粒子泡沫的第二方法变体中，同样首先借助于具有孔板的挤出机加工由90重量％至100重量％的PESU和0重量％至10重量％的添加剂组成的组合物以获得粒料，但在此没有加载发泡剂。此处同样，在进料区和螺杆尖端之间的温度—其同样不必是均匀的—在180和380℃之间的范围内。所述孔板的温度同样在300和350℃之间，和在穿过所述孔板离开时，物料温度在200和360℃之间。此处，随后在高压釜中使所述粒料加载发泡剂，使得它们然后含有在0.5重量％和10重量％之间的发泡剂。所述加载了发泡剂的粒料可然后通过卸压和/或通过加热到超过200℃的温度而发泡，从而获得粒子泡沫。
本领域技术人员原则上已知将聚合物组合物实际发泡的多种方法，其特别是在用于热塑性泡沫的方法方面可用于本发明组合物。例如，可使所述组合物在150和250℃之间的温度下和在0.1和2巴之间的压力下发泡。优选地，如果所述实际发泡不接在挤出之后进行，则其在180和230℃之间的温度下在标准压力气氛中进行。
在随后加载发泡剂的变体中，将还没有发泡剂的组合物在高压釜中在例如20和120℃之间的温度下和在例如30和100巴之间的压力下与所述发泡剂混合，并随后通过降低压力和将温度升高到发泡温度使其在所述高压釜中发泡。备选地，将与所述发泡剂混合的组合物在所述高压釜中冷却并在冷却后移出。然后可将这种组合物随后通过加热到发泡温度而发泡。这也可例如在进一步的成型下进行或与诸如插件或面层的其它元件组合进行。
更优选地，将所制备的粒子泡沫材料—无论使用的方法如何—随后与覆盖材料粘合剂粘结、缝合或熔接。“熔接”在此意思是通过组分的加热在材料之间产生粘合作用，例如通过用覆盖材料部分填充在泡沫表面处的开孔。
所述覆盖材料可以是木材、金属、装饰箔、复合材料、预浸料或其它已知材料。
在随后发泡所述PESU的情况下，例如在高压釜中加载发泡剂之后，所制备的粒子泡沫也可备选地在存在覆盖材料的情况下发泡，使得它借助于粘合剂粘结或熔接与其接合。
在其中于挤出机中进行加载发泡剂的方法变体中，也可备选地将所述PESU，当从所述挤出机离开时，施加到任选加热的模具中，其任选容纳有覆盖材料。在这种情况下，在成型的同时进行发泡，从而获得粒子泡沫或复合材料。备选地，所述组合物，当从所述挤出机离开时，可被引导到泡沫喷射设备中。在该设备中，然后直接在成型的同时进行发泡。
无论使用的变体如何，所述粒子泡沫或所述复合材料可在所述发泡过程中被提供入口，和/或可将通道引入到所述粒子泡沫中。
根据本发明的泡沫材料或者通过根据本发明的方法制备的泡沫材料可尤其用于航天器或飞机的构造中，尤其用于它们的内部。这可在此包括所述粒子泡沫，无论是否是通过根据本发明的方法制备的，以及同样包括由其实现的复合材料。更特别地，由于它们的低可燃性，本发明的泡沫材料还可被安装在这些车辆的内部空间。
此外，根据本发明制备的HT泡沫可被进一步加工以获得泡沫模制品或泡沫芯复合材料。这些泡沫模制品或泡沫芯复合材料可尤其用于批量生产，例如用于汽车工业中的车身构造或内部衬里，轨道车辆构造或造船业中的内部构件，用于航空航天工业，用于机械工程，用于运动设备的生产，用于家具构造或用于风力涡轮机的构造。

Claims (14)

1.PESU粒子泡沫用于航空工业的用途，其特征在于经发泡的PESU具有在180和215℃之间的玻璃化转变温度，和所述粒子泡沫的平均泡孔直径小于1000μm。
2.根据权利要求1的PESU粒子泡沫的用途，其特征在于所述粒子泡沫是由从80重量％至99.5重量％的PESU、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的。
3.根据权利要求2的PESU粒子泡沫的用途，其特征在于所述添加剂是阻燃剂、增塑剂、颜料、UV稳定剂、成核剂、抗冲改性剂、粘合促进剂、流变学改性剂、扩链剂、纤维和/或纳米粒子。
4.根据权利要求2或3的PESU粒子泡沫的用途，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的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PESU粒子泡沫的用途，其特征在于所述粒子泡沫满足大于0.5MPa的根据ISO1926的抗拉强度，在8％和12％之间的根据ISO1926的断裂伸长率，在室温下大于8MPa的根据ASTM C273的剪切模量，在室温下大于0.45MPa的根据ASTM C273的抗剪切强度，在室温下大于13MPa的根据ISO 844的压缩模量，和在室温下大于0.4MPa的根据ISO 844的压缩强度。
6.根据权利要求1至5中至少一项的PESU粒子泡沫的用途，其特征在于在轻质构造中的用途是在航空工业中、在造船业中、在汽车工业中或者在轨道车辆构造中的用途。
7.制备用于根据权利要求1至5中至少一项的用途的PESU粒子泡沫的方法，其特征在于将由80重量％至99.5重量％的PESU、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借助于具有孔板的挤出机加工以获得经发泡的粒料，其中在进料区和螺杆尖端之间的温度在180和380℃之间的范围内，所述孔板的温度在300和350℃之间，和当穿过所述孔板离开时，物料温度在200和360℃之间，和特征在于将经发泡的粒料随后进一步发泡以获得粒子泡沫。
8.制备用于根据权利要求1至5中至少一项的用途的PESU粒子泡沫的方法，其特征在于将由90重量％至100重量％的PESU和0重量％至10重量％的添加剂组成的组合物借助于具有孔板的挤出机加工以获得粒料，其中在进料区和螺杆尖端之间的温度在180和380℃之间的范围内，所述孔板的温度在300和350℃之间，和当穿过所述孔板离开时，物料温度在200和360℃之间，特征在于随后在高压釜中将所述粒料加载发泡剂，使得它们随后含有在0.5重量％和10重量％之间的发泡剂，和特征在于加载有发泡剂的粒料然后通过卸压和/或通过加热到超过200℃的温度而发泡，从而获得粒子泡沫。
9.制备复合材料部件的方法，其特征在于将借助于根据权利要求7或8中任一项的方法制备的粒子泡沫与覆盖材料进行粘合剂粘结、缝合或熔接。
10.制备复合材料部件的方法，其特征在于将借助于根据权利要求8的方法制备的粒子泡沫在存在覆盖材料的情况下一起发泡，使得它借助于粘合剂粘结或熔接与其接合。
11.根据权利要求7的方法，其特征在于将当从所述挤出机离开时的所述PESU引入到任选加热的模具中，该模具任选容纳有覆盖材料，并在此在成型的同时将所述PESU发泡，从而获得粒子泡沫或复合材料。
12.根据权利要求7至11中至少一项的方法，其特征在于，在发泡过程中，将入口和/或通道引入到所述粒子泡沫中。
13.根据权利要求7、8、11或12中任一项制备的粒子泡沫在飞机构造中的用途。
14.根据权利要求9、10、11或12中任一项制备的复合材料在飞机构造中的用途。
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