CN107848166B - 制造夹层板的方法 - Google Patents

制造夹层板的方法 Download PDF

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CN107848166B
CN107848166B CN201680040739.2A CN201680040739A CN107848166B CN 107848166 B CN107848166 B CN 107848166B CN 201680040739 A CN201680040739 A CN 201680040739A CN 107848166 B CN107848166 B CN 107848166B
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cooling
sandwich panel
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M·T·德格路特
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Fits Holding BV
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Abstract

本发明涉及一种制造夹层板的方法，所述方法包括以下步骤：a)提供由第一覆盖部分和第二覆盖部分以及在这些覆盖部分之间的含有物理起泡剂的热塑性材料的芯部分组成的板形组件；b)在压机中的热压具之间在压力下将从步骤a)得到的组件加热至在所述芯部分中的热塑性材料的玻璃转化温度以下的发泡温度，从而实现发泡的芯部分粘附到所述第一覆盖部分和所述第二覆盖部分；c)在压力下并在所述发泡温度下使所述芯部分中的热塑性材料发泡，其中所述压具之间的间隔被增大；d)冷却步骤：冷却从步骤c)得到的发泡的夹层板，同时使所述夹层板保持在压力下在所述压具之间；e)从所述压机移除如此冷却的夹层板；以及f)干燥如此获得的夹层板；其中所述冷却步骤d)包括以第一冷却速率将发泡的组件从所述发泡温度冷却至在70‑100℃的范围内的中间温度的第一子步骤d1)以及以第二冷却速率将发泡的组件从所述中间温度冷却至环境温度的第二子步骤d2)，所述第二冷却速率小于所述第一冷却速率。

Description

制造夹层板的方法
本发明涉及一种根据所谓的现场发泡技术(in situ foaming technique)制造夹层板的方法，所述夹层板包括在两个覆盖部分之间的发泡的芯部分。
EP636463A1已经公开了此所谓的现场发泡技术。此已知的技术包括以下步骤：提供由包括一定量的合适的物理起泡剂(泡胀剂或溶剂)的热塑性材料形成的片材；将此片材放置在由类似的热塑性材料形成的两个纤维增强的覆盖层之间；将热塑性芯和纤维增强的覆盖层的组件放置在两个热压板之间；向该组件供应热量和压力，且当达到发泡温度时，通过增加所述压板之间的间隔来引起该热塑性芯发泡，当获得预定厚度的发泡的芯时冷却所述压板，同时因此获得的夹层板被保持在压力下，随后是干燥步骤，以减少剩余的物理起泡剂或溶剂的含量。
WO2006080833A1已经公开的是，在现场发泡技术的升高温度下的干燥步骤期间，优选地移除剩余的物理起泡剂，同时限制其经由发泡的芯的周边边缘流出。
还从P.W.C.Kluit的论文“The development of in-situ foamed sandwichpanels”(代尔夫特大学出版社，1997年，第63页)已知的是，关于使用丙酮作为物理起泡剂进行PEI现场发泡的机械性能的优化参数是：
丙酮重量百分比：11.5-12.5
发泡温度：180℃
初始压力：3MPa
加热时间：20秒
压机打开速度：0.4-0.5mm/s
最终高度：10-11mm
冷却速率：100℃/分直到90℃，随后是20℃/分直到20℃
Kluit解释道，针对25×25cm夹层的实验已经示出以100℃/分从发泡温度迅速冷却到环境温度总是导致粘附劣质。基于实验结果，考虑到发泡的芯部分和覆盖部分之间的粘附强度，选择用于降低冷却速率的90℃的中间温度。尽管这些结果是有希望的，但是此粘附仍然局部很差。这在按比例扩大到较大尺寸的夹层时变得更明显。在按比例扩大时，未实现Kluit引用的强度值。
根据WO86/04017A1，一种通过起始材料的放热反应制造聚亚胺酯块或其他开孔泡沫的方法，其中一旦该反应已经达到期望的完成阶段，冷却气体就被传递通过块的主体以带走反应热量，直到达到稳定温度。
因此，本发明旨在提供一种具有根据现场发泡技术所描述的性质的夹层板，其中改善了发泡的芯部分和覆盖部分之间的粘附。
因此，根据本发明的制造夹层板的方法包括以下步骤：
a)组装步骤：提供由第一覆盖部分和第二覆盖部分以及在这些覆盖部分之间的含有物理起泡剂的热塑性材料的芯部分组成的板形组件；
b)加热步骤：在压机中的热压具之间在压力下将从步骤a)得到的组件加热至在所述芯部分中的热塑性材料的玻璃转化温度以下的发泡温度，从而实现发泡的芯部分粘附到所述第一覆盖部分和所述第二覆盖部分；
c)发泡步骤：在压力下并在所述发泡温度下使所述芯部分中的热塑性材料发泡，其中所述压具之间的间隔被增大；
d)冷却步骤：冷却从步骤c)得到的发泡的夹层板，同时使所述夹层板保持在压力下在所述压具之间；
e)卸料步骤：从所述压机移除如此冷却的夹层板；以及
f)干燥步骤：干燥如此获得的夹层板；
其中所述冷却步骤d)包括：以第一冷却速率将发泡的组件从所述发泡温度冷却至在70-100℃的范围内的中间温度的第一子步骤d1)以及以第二冷却速率将发泡的组件从所述中间温度冷却至环境温度的第二子步骤d2)，其中所述第一冷却速率是至少140℃/分且其中所述第二冷却速率小于所述第一冷却速率。
在根据本发明的方法中，首先通过将第一覆盖部分、芯部分和第二覆盖部分堆叠到彼此之上来制备板形组件，所述芯部件由含有起泡剂的热塑性材料制成，所述起泡剂的量足以发泡到在后续步骤中实现的最终厚度。通常，这些部分将作为片材或膜呈现。所述板形组件通常是柔性的且适应于压具的形状，所述压具的形状可以是平坦的以生产平坦的(平面的)夹层板。还设想了例如用于制造汽车的车顶或飞机的内侧壁板的形状更加复杂的压具，诸如弯曲的或在不同方向上双弯曲的。通常，压具(诸如平坦的压板)被可脱离地安装在压机中。
在热压板之间在加压条件下将所述组件加热至发泡温度，以防止芯部分过早膨胀，并同时使待发泡的芯部分结合到所述覆盖部分。在所述发泡温度下，以受控的方式打开所述压机，从而允许芯部分发泡。在达到由发泡的芯部分的高度确定的板的预定厚度时，根据多步骤过程冷却如此获得的夹层板。然而，相较于已知的现有技术的两步过程，在所述发泡温度和所述中间温度之间第一子步骤的冷却速率高得多。可以在从现有技术知晓的条件下执行第二子步骤。
已经显现的是，通过增大第一子步骤中的冷却速率，粘附被显著改善并且不太可能呈现局部缺陷。
可以在所述芯部分中使用任何热塑性塑料材料来执行根据本发明的方法，所述热塑性材料可以通过起泡剂来发泡。合适的热塑性材料的实施例包括聚醚酰亚胺(PEI)、聚醚砜(PES)、聚砜(PSU)、聚苯硫醚(PPS)、聚苯砜(PPSU)、聚酮、液晶聚合物、聚碳酸酯(PC)、丙烯等。用于与物理起泡剂一起使用的优选的热塑性材料是聚醚酰亚胺(PEI)。
所述芯部分包含一定量的物理起泡剂，该物理起泡剂足以将芯部分中的热塑性材料发泡至期望的最终厚度。此厚度由在所述发泡步骤c)和所述冷却步骤d)中所述压具之间实现的最终距离确定。该物理起泡剂的典型实施例包括低沸点有机化合物。优选的实施例是丙酮。
在所述发泡步骤中形成了闭孔泡沫，通常是具有在高度方向上定向的细长的孔的各向异性泡沫(也就是说，孔的最大尺寸在从一个覆盖部分到另一个覆盖部分的方向上延伸)。
所述覆盖部分可以适当地选自由热塑性材料、金属和其组合物形成的片材。适当地，覆盖部分的热塑性材料(如果有的话)与热塑性芯部分的热塑性材料相同。合适的热塑性材料包括聚醚砜(PES)、聚苯砜(PPSU)和聚砜(PSU)，尤其是聚醚酰亚胺(PEI)，鉴于上述材料的有利的滞燃性能。然而，还设想了不同的热塑性材料的组合。不同的热塑性材料的组合的合适的实施例尤其包括覆盖部分之间的PEI芯部分——其中所述覆盖部分中的至少一个由PS或PC制成——以及PES芯部分和至少一个PC覆盖部分。考虑到重量，铝是用于覆盖部分的优选的金属。考虑到重量和强度，在一个有利的实施方案中，所述第一覆盖部分和所述第二覆盖部分中的至少一个包括一个或多个纤维增强的热塑性材料的加固层。
此处注意到，如果一个覆盖部分包括多个(纤维增强的)塑料材料子层，则这些层被加固(也就是说，在加压条件下受到在玻璃转化温度以上的热处理)，使得这些(纤维增强的)热塑性子层不可逆地粘附至彼此，并形成单个整体式覆盖部分。此加固步骤是必要的，这是因为在所述发泡步骤期间在这些层之间不发生结合，原因是物理起泡剂不能够从所述芯部分穿过邻近的层扩散到所述覆盖部分的各层之间的交界上。
如果在覆盖部分中存在增强物，则玻璃纤维是增强物的一个优选实施例。然而，可以应用其他无机纤维(诸如金属纤维、碳纤维)和有机纤维(像聚芳聚酰胺纤维)。除了以上合成纤维之外，也可以使用天然纤维。覆盖部分的增强物中的纤维可以可选地被定向，且对长度和定向没有任何限制。针织织物、编织织物、垫子、布和单向纤维代表其多种的表现形式。
在与上文提及的现有技术的文献中公开的条件类似的条件下执行所述加热步骤、所述发泡步骤和所述干燥步骤，这取决于起始材料和尺寸。通常，所述加热步骤、所述发泡步骤和所述冷却步骤期间的压力在3-5MPa的范围内。还设想了较高的压力。在加热步骤b)中，所述组件被布置在压机中，所述压机优选地被预加热。当加热压具之间的组件时，所述组件的温度达到发泡温度(例如，对于PEI芯部分是175-182℃)，然后，压板之间的距离被增大至预定值。在冷却步骤d)中，发泡的组件在于压力下(通常基本上是与发泡期间相同的压力)被保持在压机中的同时被冷却至环境温度，如上文所解释的。在第一冷却步骤d1)中，以至少140℃/分、优选地200℃/分以上、更优选地大于240℃/分的冷却速率冷却夹层直到所述中间温度，例如90℃。随后，进行第二冷却处理，其中以低得多的平均冷却速率、优选地以小于所述第一冷却速率的一半的平均冷却速率、更优选地以25℃/分或更小(诸如20℃/分)的平均冷却速率从所述中间温度进一步冷却发泡的夹层板。如果所述第一冷却步骤中的冷却速率小于140℃，则粘附较差。高于200℃/分的高冷却速率，例如超过240℃/分，提供更优的结果。
在从所述压机卸载如此获得的夹层板之后，所述夹层板受到干燥处理。优选地，通过将温度间隔地增加一直到在大约150℃至大约发泡的芯热塑性材料的玻璃转化温度的范围内的温度来进行此干燥处理。对于PEI，Tg是217℃。间隔之间的温度增加通常是大约10度。所述夹层板被保持在每个中间温度达充足的时间段，例如两个小时。有利地，在所述发泡步骤b)结束之后的10-12小时内开始所述干燥步骤e)。如果所述覆盖部分中的至少一个包括热塑性材料，则优选地如WO2006/080833A1中所公开的那样来进行干燥。
使用根据本发明的方法获得的夹层板还可以被进一步处理，例如通过边缘修整而被成形为期望的最终形状。根据本发明制成的夹层板有利地被用在要求防火性能和/或充足的强度/刚度的轻重量应用中。优选的应用领域是运输部门，特别是航空业和航天业。
为了实现所述第一子步骤d1)中的高冷却速率，通常工具钢(tool steel)制成的压板被设置有平行钻孔，其中在邻近的钻孔中在相反方向上产生冷却水的强制流动。现在已经显现的是，如果在压具的平面中存在温度差(非均匀冷却)，则获得的夹层的外观可能较差，特别是冷却钻孔的位置可能作为褪色的区域被反映出来并可见。此外，覆盖部分和发泡的芯部分之间的粘附可能是不均匀的，从而在交界处而不是在发泡的芯部分内引起局部失效的风险。
因此，在子步骤d1)和d2)期间，压板之间的温度差优选地小于2℃(在所述压板的表面下方4mm测量的)。
在一些情况中，取决于诸多因素，像夹层板的尺寸、压机的构造材料、冷却能力等，已经显现出难以均匀地降低压具的温度(意味着在压具的表面上大体上不存在温度差)。在这样的条件下，已经证明设置导热系数比压机的构造材料的导热系数高的材料层是有用的。铜层或铝层(诸如由其编织的垫子)是优选的实施例。这样的垫子或片材可以被容易地布置在根据本发明的方法的步骤a)中的组件的两侧，或被插入在压机本身中。此具有高导热系数的材料层有助于在冷却期间使压机的温度均衡，从而减小压具表面上的温度变化，并减小压具之间的温度差异。此实施方案有助于均匀冷却，其结果是：在获得的夹层中没有来自压板的冷却钻孔的痕迹是可见的。
借助于下面的实施例进一步例示本发明。
实施例1
第一覆盖部分和第二覆盖部分：每个部分是用33±2％PEI浸渍并加固的一层US-style 7781玻璃织物PEI(聚醚酰亚胺)，层厚度＝0.23mm；热塑性芯部分：用12.1-12.9重量％丙酮浸渍的两个PEI((聚醚酰亚胺)Ultem 1000)膜，膜厚度在250-300微米的范围内。所述膜中的丙酮的百分比被确定为：((膜+丙酮的以g为单位的重量)减去(净膜的以g为单位的重量))除以(净膜以g为单位的重量)。
若干个FITS板(平面尺寸50×30cm)被制造为具有以下配置：
通过将两个浸渍丙酮的PEI膜作为芯部分置于相同的第一覆盖部分和第二覆盖部分之间来组装成一个对称的堆叠件，该第一覆盖部分和该第二覆盖部分各自由一个或两个如上文所指出的玻璃织物层构成。此组件被放置在压机的热压板之间。在关闭压机之后，该组件在几秒内被加热到所要求的178-180℃的发泡温度。温度测量设备(Pt元件类型K)的中心位于压板的表面下方4mm。压力为4MPa。当达到此发泡温度时，压机在将压力维持在基本上相同的值处的同时根据一定的发泡曲线被打开到最终夹层板的预定厚度(如下文所指定的)，在此之后，使压板且因此使热塑性夹层板在25秒内从所述发泡温度冷却至90℃，并以20℃/分的平均冷却速率进一步冷却至环境温度。最后，如此获得的夹层板根据WO2006080833A1经历干燥步骤，通过用带子捆扎边缘以减少丙酮的周边流出并且以在给定的温度下使用在2-4小时的间隔之间10℃的温度增加引导丙酮穿过所述覆盖部分。
以此方式，制造具有9.5mm和7.5mm的厚度的夹层板。使用根据ASTM C297的面内拉伸强度测试程序针对纤维增强的热塑性PEI覆盖部分和现场发泡的PEI芯部分之间的粘附测试所述夹层板。
具有85kg/m3的泡沫密度的9.5mm厚的现场发泡的热塑性夹层板(芯部分由两个300微米的浸渍丙酮的PEI膜制成)示出3.4MPa的平均平放拉伸强度。具有90kg/m3的泡沫密度的7.5mm厚的现场发泡的热塑性夹层板(芯部分由2个250微米的浸渍丙酮的PEI膜制成)示出3.9MPa的平均平放拉伸强度。
通常，测试样本的失效发生在热塑性芯部分中，这指示芯部分和覆盖部分之间的粘附是充足的。不能够从所述泡沫芯手动地剥落所述覆盖部分。
实施例2
第一覆盖部分和第二覆盖部分：每个部分是用33±2％PEI浸渍和加固的一层US-style 7781玻璃织物PEI(聚醚酰亚胺)，覆盖部分厚度＝0.23mm；或者每个部分是用33±2％PEI浸渍和加固的两层US-style7781玻璃织物PEI(聚醚酰亚胺)，覆盖部分厚度＝0.46mm。热塑性芯部分：用12.1-12.9重量％丙酮浸渍的三个PEI((聚醚酰亚胺)Ultem1000)膜，膜厚度为250微米。通过将热塑性芯部分置于第一覆盖部分和第二覆盖部分之间制备组件。使用相同的条件使此组件经历如实施例1中概述的现场发泡。获得具有11.3mm的厚度的夹层板(25×25cm)。具有包括浸渍有PEI的一层玻璃织物的覆盖部分的热塑性夹层板具有87kg/m3的泡沫密度且示出3.5MPa的平均平放拉伸强度。具有包括浸渍有PEI的加固的两层玻璃织物的覆盖部分的热塑性夹层板具有91kg/m3的泡沫密度且示出3.9MPa的平均平放拉伸强度。
通常，测试样本的失效发生在热塑性芯部分中，指示芯部分和覆盖部分之间的粘附是充足的。不能够从泡沫芯手动地剥落所述覆盖部分。
用50×30cm的夹层板获得相同的测试结果。
实施例3(比较)
第一覆盖部分和第二覆盖部分：每个部分是用33±2％PEI浸渍和加固的一层US-style 7781玻璃织物PEI(聚醚酰亚胺)，覆盖部分厚度＝0.23mm；或者每个部分是用33±2％PEI浸渍和加固的两层US-style7781玻璃织物PEI(聚醚酰亚胺)，覆盖部分厚度＝0.46mm。热塑性芯部分：用12.1-12.9重量％丙酮浸渍的三个PEI((聚醚酰亚胺)Ultem1000)膜，膜厚度为250微米。通过将热塑性芯部分置于第一覆盖部分和第二覆盖部分制备组件。除了使获得的夹层在40秒内从发泡温度冷却至90℃之外，如实施例1中概述的使此组件经历现场发泡。获得具有11.3mm的厚度的夹层板(25×25cm)。具有包括浸渍有PEI的一层玻璃织物的覆盖部分的热塑性夹层板具有87kg/m3的泡沫密度且示出1.8MPa的平均平放拉伸强度。具有包括浸渍有PEI的加固的两层玻璃织物的覆盖部分的热塑性夹层板具有91kg/m3的泡沫密度且示出2.3MPa的平均平放拉伸强度。
通常，测试样本的失效发生在纤维增强的热塑性覆盖部分和现场发泡的芯部分之间的交界处，指示交界处的粘附小于泡沫的强度。另外，可以相当容易地从泡沫芯手动地剥落所述覆盖部分。
用具有50×30cm的尺寸的板获得相同的测试结果。

Claims (12)

1.一种制造夹层板的方法，所述方法包括以下步骤：
a)组装步骤：提供由第一覆盖部分和第二覆盖部分以及在这些覆盖部分之间的含有物理起泡剂的热塑性材料的芯部分组成的板形组件；
b)加热步骤：在压机中的热压具之间在压力下将从步骤a)得到的组件加热至在所述芯部分中的热塑性材料的玻璃转化温度以下的发泡温度，从而实现待发泡的芯部分粘附到所述第一覆盖部分和所述第二覆盖部分；
c)发泡步骤：在压力下并在所述发泡温度下使所述芯部分中的热塑性材料发泡，其中所述压具之间的间隔被增大；
d)冷却步骤：冷却从步骤c)得到的发泡的夹层板，同时使所述夹层板保持在压力下在所述压具之间；
e)卸料步骤：从所述压机移除如此冷却的夹层板；以及
f)干燥步骤：干燥如此获得的夹层板；
其中以两个子步骤执行所述冷却步骤d)，包括：以第一冷却速率将发泡的组件从所述发泡温度冷却至在70-100℃的范围内的中间温度的第一子步骤d1)以及以第二冷却速率将发泡的组件从所述中间温度冷却至环境温度的第二子步骤d2)，其中所述第一冷却速率是至少140℃/分且其中所述第二冷却速率小于所述第一冷却速率。
2.根据权利要求1所述的方法，其中所述第一冷却速率大于200℃/20分。
3.根据权利要求1或2所述的方法，其中所述第二冷却速率小于所述第一冷却速率的一半。
4.根据权利要求1或2所述的方法，其中所述第二冷却速率是25℃/分或更小。
5.根据权利要求1或2所述的方法，其中在子步骤d1)和d2)期间，所述压具之间的温度差小于2℃。
6.根据权利要求1或2所述的方法，其中所述压具的表面设置有具有导热系数的材料层，该导热系数高于制造所述压具所用的构造材料的导热系数。
7.根据权利要求6所述的方法，其中具有较高导热系数的该材料层是由铜或铝制成的层。
8.根据权利要求1或2所述的方法，其中所述第一覆盖部分和所述第二覆盖部分中的至少一个包括热塑性材料层。
9.根据权利要求8所述的方法，其中覆盖部分的热塑性材料选自如下一组：聚醚酰亚胺、聚醚砜、聚苯砜和聚砜。
10.根据权利要求1或2所述的方法，其中所述芯部分的热塑性材料是聚醚酰亚胺。
11.根据权利要求1或2所述的方法，其中所述物理起泡剂是丙酮。
12.根据权利要求8所述的方法，其中所述第一覆盖部分和所述第二覆盖部分中的至少一个包括纤维增强的热塑性材料层。
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