CN113710472A - 具有阻燃特性的轻质夹层结构及其制造方法 - Google Patents

具有阻燃特性的轻质夹层结构及其制造方法 Download PDF

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Publication number
CN113710472A
CN113710472A CN202080029228.7A CN202080029228A CN113710472A CN 113710472 A CN113710472 A CN 113710472A CN 202080029228 A CN202080029228 A CN 202080029228A CN 113710472 A CN113710472 A CN 113710472A
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China
Prior art keywords
thermoplastic
mol
polymer
fibers
foam core
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CN202080029228.7A
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English (en)
Inventor
S·摩塔拉
P·沃洛森
P·托尼奥洛
F·伦兹
A·沃格尔
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Cytec Industries Inc
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Cytec Industries Inc
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Publication of CN113710472A publication Critical patent/CN113710472A/zh
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Abstract

披露了一种轻质的、阻燃的多层复合结构，其至少具有以下部件：具有两个相反表面的热塑性泡沫芯；在该泡沫芯的这些相反表面的至少一个上的热塑性粘合剂膜，在每个粘合剂膜上的一个或多个复合层。该一个或多个复合层由嵌入热塑性聚合物或热固性树脂基质中的增强纤维构成。粘合剂结合通过在该热塑性泡沫芯与相邻复合层之间插入的交错的热塑性粘合剂膜实现。该热塑性粘合剂膜由热塑性聚合物组合物形成，该热塑性聚合物组合物具有的Tg比泡沫芯材料的Tg低至少20℃。

Description

具有阻燃特性的轻质夹层结构及其制造方法
本披露总体上涉及具有热塑性泡沫层的轻质复合材料、这些材料的应用和用于制造此类结构的方法。
附图说明
图1示出了具有热塑性泡沫芯的示例性夹层结构。
图2示出了用于制造夹层结构的具有双带压机系统的示例性装置。
图3示出了在暗场光中以x100放大倍率拍摄的对照夹层板的界面的抛光图像，其中对照夹层板是根据本文披露的实例1制造的。
图4示出了在暗场光中以x100放大倍率拍摄的另一个夹层板的界面的抛光图像，其中夹层板是根据本文披露的实例2制造的。
具体实施方式
具有热塑性泡沫芯的复合夹层结构已经用于飞机的内部结构，如舱门和壁板。此类夹层结构提供强度和刚度，同时最小化结构的重量。虽然飞机的内部复合零件不要求如机身和机翼等主要结构的结构性能，但这些零件仍有其自身一套苛刻的要求，这些要求包括低重量下的刚度和强度、尺寸稳定性、持久美观性、对清洁溶剂的耐化学性、以及在火焰、烟雾和毒性(FST)标准和热释放速率(HRR)标准方面的严格的阻燃标准。
由热塑性材料构成的多层复合结构的制造是困难的，因为需要高温和高压来确保各种热塑性层的良好结合。制造在外皮层之间具有热塑性泡沫芯的夹层结构存在的一个挑战是，在不使用高固结压力(其将导致泡沫芯坍塌)的情况下，在芯层与皮层之间获得良好的结合的能力。
在将蜂窝或泡沫芯结合到外皮层的常规方法中，整个夹层板组件行进通过加热区，由此在压力(典型地由加热的压板施加)下将夹层板加热至结合温度。如果使用热塑性芯，如果结合所需的温度超过芯材料的玻璃化转变温度(Tg)并且如果压力过高，则会发生芯坍塌或变形。这种坍塌或变形是由于从压板通过外皮向芯过度传热(从而使泡沫芯的温度升高超过热塑性芯材料的Tg)和通过压板施加的压力的组合。
本披露的一个方面涉及一种轻质的、阻燃的多层复合结构，其至少具有以下部件：具有两个相反表面的热塑性泡沫芯；在泡沫芯的相反表面的至少一个上的热塑性粘合剂膜，在每个粘合剂膜上的一个或多个复合层。粘合剂结合通过在热塑性泡沫芯与相邻复合层之间插入的交错的热塑性粘合剂膜实现。复合层由嵌入热塑性聚合物或热固性树脂基质中的增强纤维构成。热塑性泡沫芯由具有如通过差示扫描量热法(DSC)以5℃/min的加热速率确定的至少200℃、优选210℃至240℃的玻璃化转变温度(Tg)的发泡热塑性材料形成，并且热塑性粘合剂膜由热塑性聚合物组合物形成，该组合物具有的Tg至少比发泡热塑性材料的Tg低20℃。
在优选的实施例中，多层复合结构是夹层结构，其中热塑性泡沫芯以片材形式插入两个外皮之间。图1示出了示例性夹层结构，其包括热塑性泡沫芯10、交错的粘合剂膜11A和11B、外皮12A和12B，其中每个外皮由多个复合层或单个复合层的层压物(或叠层)构成。皮的复合层可以彼此相同或不同。此外，热塑性泡沫芯没有任何增强纤维，如碳纤维、玻璃纤维和聚合物纤维，或者任何延伸穿过其厚度的孔。
在优选的实施例中，选择在夹层结构中的泡沫芯和皮材料，使得该结构符合对于材料的FAR/JAR/CS 23.853“Passenger and crew compartment interiors[乘客和工作人员舱内部]”和23.855“Cargo and baggage compartment fire protection[货物和行李舱防火]”易燃性要求。
用于将热塑性泡沫芯结合到一个或多个复合层的所选择的热塑性粘合剂在粘合剂断裂韧性和剥离强度方面提供了优异结合。此外，发现使用粘合剂热塑性膜(具有的玻璃化转变温度比泡沫芯材料的玻璃化转变温度低约20℃)提供了与连续低压双带方法(允许高生产速度)相容的夹层结构。与在层压期间需要外部热源的常规方法相比，双带方法不需要这样的外部热源来熔化皮与热塑性泡沫芯之间的交错的粘合剂层。通过带和皮材料传递到下面的粘合剂膜的热量足以熔化粘合剂膜，而不会导致皮变形或泡沫芯塌陷。
热塑性泡沫芯
在本披露的上下文中，术语“泡沫”以本领域技术人员通常已知的含义使用。参考IUPAC,Compendium of Chemical Terminology[化学术语汇编],第2版(由A.D.McNaught和A.Wilkinson编辑的"Gold Book[金皮书]".Blackwell Scientific Publications,Oxford[布莱克韦尔科学出版公司，牛津大学]1997,XML在线修正版本：由M.Nic,J.Jirat,B.Kosata创建的http://goldbook.iupac.org(2006)；由A.Jenkins编辑的更新内容.ISBN0-9678550-9-8.doi:10.1351/goldbook)，术语“泡沫”指示这样的分散体，在该分散体中按体积计大比例的气体以气泡的形式分散在液体、固体或凝胶中。气泡的直径通常大于1μm，但在气泡之间的薄层的厚度经常在通常的胶体尺寸范围内。
作为非限制性实例，基于组合物的总体积，根据本披露的发泡热塑性材料的体积的至少50％，例如至少60％、至少70％、至少80％或至少90％可以被气体占据。
泡沫芯可以具有从20至1000kg/m3、从30至800kg/m3、从35至500kg/m3、从40至300kg/m3、或从45至200kg/m3的密度。在优选的实施例中，泡沫芯具有从45至150kg/m3、并且更优选从45至80kg/m3的密度。可以根据ASTM D1622测量密度。
根据一个实施例，泡沫芯具有低于1000μm、低于500μm、低于300μm或低于250μm的平均泡孔尺寸。可以使用光学电子显微镜或扫描电子显微镜测量泡孔尺寸。
泡沫芯可以具有在3mm至50mm范围内，在一些实施例中，5mm至25mm的范围内的厚度。
本文披露的多层复合结构的泡沫芯由含有至少一种选自以下的聚合物的可发泡组合物形成：聚(芳基醚砜)(PAES)、特别是聚醚砜(PES)、聚醚醚砜(PEES)、聚(联苯基醚砜)(PPSU)；聚酰胺(PA)；聚酰亚胺(PI)；聚醚酰亚胺(PEI)；及其共聚物。通常，具有的Tg在201℃至290℃范围内的PAES聚合物适用于本文披露的目的。在一些实施例中，可发泡组合物含有不同热塑性聚合物的组合。不同PAES聚合物之间的Tg差异是由于聚合物主链结构的差异。
出于本披露的目的，“聚(芳基醚砜)(PAES)”表示其至少50mol.％的重复单元是具有式(K)的重复单元(RPAES)的任何聚合物，该mol.％是基于该聚合物中重复单元的总摩尔数：
Figure BDA0003305745280000041
其中
R，在每个位置处，独立地选自由以下组成的组：卤素、烷基、烯基、炔基、芳基、醚、硫醚、羧酸、酯、酰胺、酰亚胺、碱金属或碱土金属磺酸盐、烷基磺酸酯、碱金属或碱土金属膦酸盐、烷基膦酸酯、胺和季铵；
对于每个R，h独立地为零或范围从1至4的整数，并且
T选自由键、砜基[-S(＝O)2-]、以及基团-C(Rj)(Rk)-组成的组，其中Rj和Rk彼此相同或不同，选自氢、卤素、烷基、烯基、炔基、醚、硫醚、羧酸、酯、酰胺、酰亚胺、碱金属或碱土金属磺酸盐、烷基磺酸酯、碱金属或碱土金属膦酸盐、烷基膦酸酯、胺和季铵。
T优选地是键、砜基或基团-C(Rj)(Rk)-，其中Rj和Rk优选地是甲基。
聚(联苯基醚砜)(PPSU)特别适合作为用于泡沫芯的材料。出于本披露的目的，聚(联苯基醚砜)聚合物(PPSU)表示含有至少50mol.％的具有式(K)的重复单元(RPPSU)的任何聚合物，该mol.％是基于该聚合物中的总摩尔数：
Figure BDA0003305745280000042
其中
R，在每个位置处，独立地选自由以下组成的组：卤素、烷基、烯基、炔基、芳基、醚、硫醚、羧酸、酯、酰胺、酰亚胺、碱金属或碱土金属磺酸盐、烷基磺酸酯、碱金属或碱土金属膦酸盐、烷基膦酸酯、胺和季铵；并且
对于每个R，h独立地是零或范围从1至4的整数(例如1、2、3或4)。
根据实施例，R在上式(K)中的每个位置处，独立地选自由以下组成的组：任选地包含一个或多于一个杂原子的C1-C12部分；磺酸和磺酸盐/酯基团；膦酸和膦酸盐/酯基团；胺和季铵基团。
根据实施例，对于每个R，h是零。换句话说，根据此实施例，重复单元(RPPSU)是具有式(K’)的单元：
Figure BDA0003305745280000051
根据实施例，PPSU中至少60mol.％、至少70mol.％、至少80mol.％、至少90mol.％、至少95mol.％、至少99mol.％或所有的重复单元是具有式(K)和/或式(K’)的重复单元(RPPSU)。
根据实施例，PPSU聚合物含有至少50mol.％的具有式(L)的重复单元(RPPSU)：
Figure BDA0003305745280000052
(该mol.％是基于聚合物中的总摩尔数)。
因此，本披露的PPSU聚合物可以是均聚物或共聚物。如果它是共聚物，则它可以是无规共聚物、交替共聚物或嵌段共聚物。
根据优选的实施例，PPSU中至少60mol.％、至少70mol.％、至少80mol.％、至少90mol.％、至少95mol.％、至少99mol.％或所有的重复单元是具有式(L)的重复单元(RPPSU)。
当PPSU是共聚物时，其重复单元是以下项的混合物：上述重复单元(RPPSU)和不同于RPPSU的重复单元(R*)，如具有以下式(M)、(N)和/或(O)的单元：
Figure BDA0003305745280000061
其中
R，在每个位置处，独立地选自卤素、烷基、烯基、炔基、芳基、醚、硫醚、羧酸、酯、酰胺、酰亚胺、碱金属或碱土金属磺酸盐、烷基磺酸酯、碱金属或碱土金属膦酸盐、烷基膦酸酯、胺和季铵；并且
对于每个R，i独立地是零或范围从1至4的整数(例如1、2、3或4)。
根据实施例，R在上式(M)至(O)中的每个位置处，独立地选自由以下组成的组：任选地包含一个或多于一个杂原子的C1-C12部分；磺酸和磺酸盐/酯基团；膦酸和膦酸盐/酯基团；胺和季铵基团。
根据实施例，对于式(M)、(N)或(O)的每个R，i为零，并且重复单元R*选自下式(M’)、(N’)和(O’)：
Figure BDA0003305745280000071
根据一些实施例，PPSU中小于40mol.％、小于30mol.％、小于20mol.％、小于10mol.％、小于5mol.％、小于1mol.％或所有的重复单元是具有式(M)、(N)、(O)、(M’)、(N’)和/或(O’)的重复单元。
根据一个实施例，PPSU是具有上述重复单元(RPPSU)和不同于RPPSU的重复单元(R*)的混合物的共聚物，其中R*选自下式(M”)、(N”)和(O”)：
Figure BDA0003305745280000072
根据一些实施例，PPSU中小于45mol.％、小于40mol.％、小于35mol.％、小于30mol.％、小于20mol.％、小于10mol.％、小于5mol.％、小于1mol.％或所有的重复单元是具有式(M”)、(N”)和/或(O”)的重复单元。
用于本文目的的PPSU可以是PPSU均聚物与至少一种如上所述的PPSU共聚物的共混物。
本文披露的PPSU聚合物可以通过本领域已知的任何方法制备。例如，PPSU聚合物可以是4,4’-二羟基联苯(双酚)和4,4’-二氯二苯砜缩合的结果。单体单元的反应通过亲核芳香族取代同时消除一个作为离去基团的卤化氢单元进行。然而，应注意，所得聚(联苯基醚砜)的结构不取决于离去基团的性质。
缺陷、端基和单体的杂质可以以非常少量结合在本披露的(共)聚合物PPSU中，从而有利地没有负面地影响其性能。
出于本文披露的目的，合适的PPSU的实例是从美国索尔维特种聚合物有限公司(Solvay Specialty Polymers USA,L.L.C.)可商购的
Figure BDA0003305745280000081
PPSU。
在优选的实施例中，热塑性发泡芯是具有的Tg在210℃-240℃范围内的发泡材料，并且由含有聚(联苯基醚砜)聚合物(PPSU)作为主要组分(即，基于组合物的总重量，PPSU以大于50wt.％(重量百分比)、或大于80wt.％的量存在)的可发泡组合物形成。PPSU的重均分子量(Mw)可以是从30,000至90,000g/mol，例如从40,000至80,000g/mol或从50,000至70,000g/mol。
PAES(包括PPSU和PSU)的重均分子量(Mw)可以通过凝胶渗透色谱法(GPC)使用亚甲基氯作为流动相(来自安捷伦科技公司(Agilent Technologies)的带有保护柱的2x 5μ混合D柱；流速：1.5mL/min；注射体积：20μL的0.2w/v％样品溶液)用聚苯乙烯标准物确定。
更精确地，可以通过凝胶渗透色谱法(GPC)使用亚甲基氯作为流动相来测量PAES聚合物的重均分子量(Mw)。可以例如使用以下详述的方法：使用两个来自安捷伦科技公司的带有保护柱的5μ混合D柱进行分离。使用254nm的紫外检测器获得色谱图。选择1.5ml/min的流速和20μL注射体积的在流动相中的0.2w/v％溶液。使用12种窄分子量聚苯乙烯标准物(峰分子量范围：371,000至580g/mol)进行校准。
除了上述热塑性聚合物(例如PAES)之外，用于形成泡沫芯的可发泡组合物可以进一步包含最高达10wt.％(基于聚合物组合物的总重量)的至少一种添加剂(AD)。该添加剂可以选自：成核剂、化学发泡剂或其残余物；UV吸收剂；稳定剂(如光稳定剂和其他)；润滑剂；增塑剂；颜料；染料；着色剂；抗静电剂；金属减活剂；及其混合物。
抗氧化剂的实例是亚磷酸酯、磷酸酯、受阻酚、或其混合物。还可以添加表面活性剂来帮助气泡成核并且使这些气泡在发泡过程的气泡生长阶段期间稳定。
在一些实施例中，可发泡组合物含有一种或多种成核剂。成核剂通过提供气泡形成位点而有助于控制泡沫结构。成核剂的实例是玻璃纤维、碳纤维、石墨纤维、碳化硅纤维、芳纶纤维、硅灰石、滑石、云母、粘土、碳酸钙、二氧化钛、钛酸钾、二氧化硅、硅酸盐、高岭土、白垩、矾土、铝酸盐、氮化硼和氧化铝。
可发泡组合物可以进一步包含一种或多种无机颜料。添加无机颜料以通过改变反射或透射光的颜色(作为波长选择吸收的结果)来获得组合物的所选择的外观。无机颜料的实例是二氧化钛、硫化锌、氧化锌、氧化镁、硫酸钡、炭黑、磷酸钴、钛酸钴、硫硒化镉、硒化镉、酞菁铜、群青、群青紫、铁酸锌、铁酸镁和氧化铁。
基于组合物的总重量，可发泡组合物可以含有从0.1至9wt.％、从0.2至5wt.％、或从0.5至2wt.％的至少一种添加剂(AD)。根据一个实施例，基于组合物的总重量，在可发泡组合物中含有从0.1至9wt.％、从0.2至5wt.％、或从0.5至3wt.％的至少一种成核剂。
发泡方法可以是化学的或物理的发泡方法。当发泡方法是化学发泡方法时，可以使用化学发泡剂、特别是化学起泡剂。化学发泡剂总体上指的是在发泡条件下在热影响下分解或反应以生成发泡气体的那些组合物。可以将化学发泡剂添加到聚合物组合物中以原位产生发泡气体。化学发泡也可以在挤出装置中实现。
热塑性粘合剂
在一些实施例中，本文披露的用于结合目的的热塑性粘合剂膜由聚合物组合物形成，该聚合物组合物含有至少80wt.％(重量百分比)的具有的Tg小于200℃的一种或多种聚砜(PSU)，例如，基于膜的总重量，至少85wt.％、或至少90wt.％、或至少95wt.％的PSU。粘合剂膜可以具有在25至250微米(μm)范围内、例如，在30至220μm范围内或在35至200μm范围内的厚度。
优选的聚砜(PSU)具有至少50mol.％的以下重复单元，这些重复单元是具有下式(U)的重复单元(RPSU)：
Figure BDA0003305745280000101
(该mol.％是基于该聚合物中的重复单元的总摩尔数)。
根据实施例，PSU中至少60mol.％(基于该聚合物中重复单元的总摩尔数)、至少70mol.％、至少80mol.％、至少90mol.％、至少95mol.％、至少99mol.％或全部的重复单元是具有式(U)的重复单元(RPSU)。
PSU聚合物可以是均聚物或共聚物。如果该PSU聚合物是共聚物，则它可以是无规、交替或嵌段共聚物。
当聚砜(PSU)是共聚物时，它可以包含不同于重复单元(RPSU)的并且除了该重复单元以外的重复单元(RA)，如具有式(M)、(N)和/或(O)的重复单元：
Figure BDA0003305745280000102
Figure BDA0003305745280000111
合适的可商购的PSU是来自美国索尔维特种聚合物有限公司的
Figure BDA0003305745280000112
PSU。
在优选的实施例中，粘合剂膜由PSU聚合物形成，其中PSU聚合物中至少90mol.％或所有的重复单元是具有式(U)的重复单元(RPSU)，并且该聚合物具有约185℃的Tg。
如通过如上所述的GPC确定的，PSU的重均分子量(Mw)可以是从30,000至110,000g/mol，例如从40,000至100,000g/mol或从50,000至90,000g/mol。
聚砜聚合物可以通过多种方法生产。例如，美国专利号4,108,837和4,175,175描述了聚芳醚并且特别是聚芳醚砜的制备。这些专利中描述了若干一步法和两步法，将这些专利以其全文通过援引方式并入本文。在这些方法中，使二元酚的碱金属复盐与二卤代苯型化合物在砜或亚砜溶剂的存在下在基本上无水的条件下反应。在两步法中，二元酚通过在砜或亚砜溶剂的存在下与碱金属或碱金属化合物反应首先原位转化为碱金属盐衍生物。在PSU制造的情况中，起始单体是双酚A和4,4’-二卤二苯砜、典型地4,4’-二氯二苯砜。双酚A首先通过首先与碱像氢氧化钠(NaOH)以1:2化学计量摩尔比反应以生产双酚A的二钠盐而转化为二碱金属盐衍生物。然后在第二步骤中使双酚A的此二钠盐与4,4’-二氯二苯砜反应以生产该聚合物。氯化钠盐作为该聚合反应的副产物而产生。
复合层
在一些实施例中，多层复合结构中的复合层含有嵌入热塑性聚合物基质中的增强纤维。
如本披露中所使用的，术语“嵌入”意指被牢固地固定在周围物质中，并且术语“基质”意指大量的材料，例如聚合物，其中封入或嵌入了某种物质。
热塑性聚合物基质包括一种或多种热塑性聚合物，该聚合物可以是无定形的或半结晶的。一种或多种热塑性聚合物整个地构成了聚合物基质的主要组分，或者大于50wt.％、例如80-100wt.％的聚合物基质由一种或多种热塑性聚合物构成。合适的热塑性聚合物包括但不限于：聚(芳基醚砜)(PAES)、特别是聚醚砜(PES)、聚醚醚砜(PEES)、聚(联苯基醚砜)(PPSU)；聚酰胺(PA)；聚酰亚胺(PI)；聚醚酰亚胺(PEI)；聚(芳基醚酮)(PAEK)聚合物，如聚醚酮酮(PEKK)、聚醚醚酮(PEEK)、聚醚酮酮(PEKK)；聚邻苯二甲酰胺(PPA)；热塑性聚氨酯；聚(甲基丙烯酸甲酯)(PMMA)；聚苯硫醚(PPS)；聚苯醚(PPO)；及其共聚物。
通常，具有的Tg在201℃至290℃范围内的PAES聚合物适用于本文披露的目的。在一些实施例中，热塑性聚合物基质含有大于50wt.％(例如80-100wt.％)的以上关于发泡热塑性材料描述的PPSU聚合物。
在其他实施例中，复合层含有嵌入热固性树脂基质中的增强纤维，该基质在热固化时硬化。优选地，热固性树脂基质含有至少一种环氧树脂、优选不同环氧树脂的共混物、和至少一种固化剂。环氧树脂和固化剂的组合构成了热固性树脂基质的大于50wt.％(例如60wt％-100wt.％)。
合适的环氧树脂包括芳香族二胺、芳香族单伯胺、氨基苯酚、多元酚、多元醇、多元羧酸的多缩水甘油基衍生物。合适的环氧树脂的实例包括双酚诸如双酚A、双酚F、双酚C、双酚S和双酚K的多缩水甘油醚；和基于甲酚和苯酚的酚醛清漆的多缩水甘油醚。
具体实例是4,4'-二氨基二苯基甲烷(TGDDM)的四缩水甘油基衍生物、间苯二酚二缩水甘油醚、三缩水甘油基-对-氨基苯酚、三缩水甘油基-间-氨基苯酚、溴双酚F二缩水甘油醚、二氨基二苯基甲烷的四缩水甘油基衍生物、三羟基苯基甲烷三缩水甘油醚、苯酚-甲醛酚醛清漆的多缩水甘油醚、邻甲酚酚醛清漆的多缩水甘油醚或四苯基乙烷的四缩水甘油醚。
可商购的环氧树脂包括N,N,N',N’-四缩水甘油基二氨基二苯基甲烷(例如来自亨斯迈公司(Huntsman)的MY 9663、MY 720和MY 721)；N,N,N',N'-四缩水甘油基-双(4-氨基苯基)-1,4-二异丙基苯(例如来自迈图公司(Momentive)的EPON 1071)；N,N,N',N'-四缩水甘油基-双(4-氨基-3,5-二甲基苯基)-1,4-二异丙基苯(例如来自迈图公司的EPON 1072)；对氨基苯酚的三缩水甘油醚(例如来自亨斯迈公司的MY 0510)；间氨基苯酚的三缩水甘油醚(例如来自亨斯迈公司的MY 0610)；基于双酚A的材料，如2,2-双(4,4'-二羟基苯基)丙烷的二缩水甘油醚(例如来自陶氏公司(Dow)的DER 661或来自迈图公司的EPON 828，以及优选在25℃下粘度为8-20Pa·s的酚醛清漆树脂；苯酚酚醛清漆树脂的缩水甘油醚(例如来自陶氏公司的DEN 431或DEN 438)；基于二环戊二烯的苯酚酚醛清漆(例如来自亨斯迈公司的Tactix 556)；1,2-邻苯二甲酸二缩水甘油酯(例如GLY CEL A-100)；二羟基二苯基甲烷(双酚F)的二缩水甘油基衍生物(例如来自亨斯迈公司的PY 306)。其他合适的环氧树脂包括环脂族化合物，诸如3',4'-环氧环己基-3,4-环氧环己烷羧酸酯(例如来自亨斯迈公司的CY179)。
固化剂适当地选自已知的固化剂，例如芳香族或脂肪族胺或胍衍生物。具体的实例是3,3'-和4,4'-二氨基二苯基砜(DDS)；亚甲基二苯胺；双(4-氨基-3,5-二甲基苯基)-1,4-二异丙基苯；双(4-氨基苯基)-1,4-二异丙基苯；4,4'亚甲基双-(2,6-二乙基)-苯胺(来自龙沙公司(Lonza)的MDEA)；4,4'亚甲基双-(3-氯,2,6-二乙基)-苯胺(来自龙沙公司的MCDEA)；4,4'亚甲基双-(2,6-二异丙基)-苯胺(来自龙沙公司的M-DIPA)；3,5-二乙基甲苯-2,4/2,6-二胺(来自龙沙公司的D-ETDA 80)；4,4'亚甲基双-(2-异丙基-6-甲基)-苯胺(来自龙沙公司的M-MIPA)；4-氯苯基-N,N-二甲基-脲(例如Monuron)；3,4-二氯苯基-N,N-二甲基-脲(例如敌草隆(Diuron))和双氰胺(例如来自太平洋锚化学公司(Pacific AnchorChemical)的
Figure BDA0003305745280000131
CG 1200)。
热固性树脂基质可以进一步含有其他添加剂，如催化剂、共聚单体、流变控制剂、增粘剂、无机或有机填充剂、作为增韧剂的热塑性和/或弹性体聚合物、核-壳橡胶颗粒、UV稳定剂/添加剂、粘度改性剂/流动控制剂、稳定剂、抑制剂、颜料、染料、阻燃剂、反应性稀释剂、以及本领域技术人员熟知的用于改性固化之前或之后的基质树脂的特性的其他添加剂。
用于热固性树脂基质的合适的增韧剂包括但不限于单独或与以下各项组合的均聚物或共聚物：聚酰胺、共聚酰胺、聚酰亚胺、芳族聚酰胺、聚酮、聚醚酰亚胺(PEI)、聚醚酮(PEK)、聚醚酮酮(PEKK)、聚醚醚酮(PEEK)、聚醚砜(PES)、聚醚醚砜(PEES)、聚酯、聚氨酯、聚砜、多硫化物、聚苯醚(PPO)和改性的PPO、聚(环氧乙烷)(PEO)和聚环氧丙烷、聚苯乙烯、聚丁二烯、聚丙烯酸酯、聚甲基丙烯酸酯、聚丙烯酸化物、聚苯砜、高性能烃聚合物、液晶聚合物、弹性体和链段弹性体。
如果添加增韧剂，则基于热固性树脂基质的总重量，此类组分以小于20wt.％的量存在。
例如，热固性树脂基质可以还包括各种阻燃剂和烟雾抑制剂以赋予特定的阻燃特性。此类抑制剂的实例是金属氧化物、三水合氧化铝(ATH)、硼酸锌如
Figure BDA0003305745280000141
ZB(从美国加利福尼亚州博伦的美国硼砂公司(U.S.Borax Inc.,Boron,California USA)可商购)、聚磷酸铵、聚磷腈、磷改性的环氧化物。如果存在的话，以上提及的添加剂的量可以是基于该树脂基质的总重量最高达35wt.％。
复合层的增强纤维可以呈短切或连续纤维、由多条长丝构成的丝束、连续单向纤维、随机取向的纤维的非织造垫/面纱、织造或非织造织物的形式。非织造织物包括不卷曲织物，该不卷曲织物含有通过缝合固定在位的单向纤维。如本文所用的术语“单向”意指在同一方向上平行对齐。
增强纤维包括碳纤维或石墨纤维，玻璃纤维，以及由碳化硅、氧化铝、硼、石英和陶瓷形成的纤维，以及由聚合物(例如像聚烯烃、聚(苯并噻唑)、聚(苯并咪唑)、聚芳酯、聚(苯并噁唑)、芳香族聚酰胺、聚芳基醚等)形成的纤维，并且可以包括具有两种或更多种此类纤维的混合物。在一些实施例中，纤维选自玻璃纤维、碳纤维、和芳香族聚酰胺纤维，如以商品名KEVLAR销售的纤维。
基于复合层的总重量，每个复合层可以含有30wt.％至60wt.％、或35wt％至50wt.％的热塑性聚合物或热固性树脂基质。每个复合层的总面积重量可以在200gsm(g/m2)至2000gsm、在一些优选的实施例中，450gsm至600gsm的范围内。
制造方法
本文披露的多层复合结构的部件通过施加热量和压力来组装和固结，以产生结合的结构。可以使用施加热量和压力的任何常规手段，如加热板或加热辊。在优选的实施例中，多层复合结构的固结通过将该结构穿过双带压机来进行。在多层复合结构穿过双带压机期间的此类固结可以在200℃至260℃范围内的温度下进行1至10分钟的时间段。
图2示出了具有双带压机的连续加工机器的实例，该机器适用于将泡沫芯、粘合剂膜和外皮的组件固结以形成集成板。参考图2，加工机器包括上部环形带20、下部环形带21、加热区中的多个加热元件22、用于调整距离的轧辊23、用于调整最终形状的S辊24、冷却区中的多个冷却元件25、在冷却区下游的修边器26、可选的截面切割器27和可选的堆叠机构28。环形带以相反方向旋转，其相互面对的侧面相互挤压，并且挤压在这些带之间通过的材料(M)。加热和冷却元件定位成与这些带的将与在这些带之间通过的材料接触的部分相邻。这种类型的双带压机系统的一个优点是，可以在低压(例如小于5巴)下进行泡沫芯夹层结构固结，由此避免泡沫芯变形或坍塌。环形带可以由不粘的弹性材料(如PTFE)或耐高温且不粘的不锈钢制成。在优选的实例中，具有不粘的不锈钢带的双带压机用于提供改进的夹层表面精加工。
在优选的实施例中，多层复合结构的制造以连续等容方法进行，该方法包括：
(a)形成至少具有以下部件的多层组件：具有两个相反表面的热塑性泡沫芯；在热塑性泡沫芯的相反表面的一个或两个上的热塑性粘合剂膜；在每个热塑性粘合剂膜上的纤维增强复合材料的一个或多个层；
(b)以0.5至5m/min的线速度使组件在双带压机的两条环形带之间通过，其中环形带之间的距离在从3mm至40mm的范围内，并且比组件在(a)时在其通过双带压机之前的组合厚度小1mm至10mm。
(c)在夹层结构通过双带压机期间将其加热至200℃至260℃范围内的温度持续1至10分钟的时间段。
热塑性泡沫芯、热塑性粘合剂膜和复合层是如上所述的。
多层组件可以就在进入双带压机之前，通过从供料辊上退绕连续的复合材料片材并且将其放置在输送机上而将其放在一起。一个或多个附加的复合材料片材可以由一个或多个附加的供料辊供应，并且放置在先前铺设的复合材料片材上。然后将在其上具有粘合剂膜的呈片材形式的热塑性泡沫芯置于复合材料的片材上，使得粘合剂膜与复合材料的片材接触。为了形成复合材料的第二外皮，将从一个或多个附加的供料辊上退绕的一个或多个复合材料上片材放置在泡沫芯片材的顶部。在这种情况下，泡沫芯片材在其上表面和下表面的每一个上具有先前施加的粘合剂膜。
在一个实施例中，连续等容方法配备有辊毯模块(Roller Carpet Module)(RCM)用于对遍及材料的整个长度和宽度的厚度进行精细和分布式控制。RCM包括顶部和底部二者上的几个小辊，这些辊与连续钢带接触(遍及钢带的整个宽度提供非常均匀的厚度控制)。在另一个实施例中，连续等容方法进一步配备有压延机模块(CAM)，该模块包括可以在钢带上施加更强压力的上部和下部压延辊，用于控制材料的厚度，其中遍及材料的整个长度和宽度都具有耐高压性。在一个优选的实施例中，由配备有辊毯模块(RCM)的机器施用连续等容方法，用于更好地精确控制泡沫并且然后控制夹层厚度。
在另一个实施例中，多层复合结构的制造以连续等压方法进行，该方法包括：
(a)形成如上所述的多层组件；
(b)以0.5至5m/min的线速度，在小于5巴的正压力(例如，从1至2巴)下使组件在双带压机的两条环形带之间通过；以及
(c)在组件通过双带压机期间将其加热至200℃至260℃范围内的温度持续1至10分钟的时间段。
实例
实例1
通过等容方法的具有未增强热塑性皮的对照板
组装了具有17.5mm厚度的
Figure BDA0003305745280000161
泡沫芯、两个PPSU R-5100树脂膜层(每个具有63μm的厚度)作为顶部和底部皮、以及在每个皮与泡沫芯之间约70gsm的BostikSPA145FR-A
Figure BDA0003305745280000162
的粘合剂膜的夹层板。Bostik SPA145FR-A
Figure BDA0003305745280000164
是阻燃聚酯网粘合剂。
Figure BDA0003305745280000163
是具有53Kg/m3密度的具有闭孔的PPSU基热塑性泡沫芯。
使所组装的板通过双带连续机器，该机器具有两条相对的环形PTFE带和12延米的加热加工区。通过将加热区的温度设置在220℃，并且使用1m/min的线速度进行所组装的夹层板的结合和固结。两个相对的环形带之间的距离等于11.8mm。
在图3中示出了所得的固结夹层板的截面，在暗场光中以x100放大倍率拍摄的皮/芯界面的抛光图像。板示出了在泡沫芯与PPSU外皮层之间的弱结合线，并且其在切割操作期间容易地解结合。
根据EN 2243-3，使固结夹层板试样经受爬鼓剥离测试(Climb Drum Peelingtest)(以25mm/min施加张力)。测试结果示出低于10N/75mm的平均剥离强度。
实例2
通过等容方法的具有未增强热塑性皮的板
与实例1一样组装两个夹层板，但是使用100μm的PSU树脂膜作为泡沫芯与两个PPSU皮层中的每一个之间的粘合剂膜。
使每个夹层板通过实例1的双带连续机器，其中在一种情况下将加热温度设置在220℃，并且在第二种情况下将加热温度设置在250℃，并且在两种情况下均使用1m/min的线速度。在这两种情况下，两个相对的环形带之间的距离等于11.8mm。
如从图4(在暗场光中以x100放大倍率拍摄的芯/皮界面的抛光图像)中可以看出两个所得的固结夹层板示出在热塑性膜粘合剂与芯之间的良好的结合。
根据EN 2243-3，使固结夹层板试样经受爬鼓剥离测试(以25mm/min施加张力)。测试结果示出，对应地，在220℃下制造的夹层的平均剥离强度是260N/75mm，并且在250℃下制造的夹层的平均剥离强度是344N/75mm。这些值明显大于实例1中对照夹层板获得的剥离强度值，其中Bostik SPA145FR-A
Figure BDA0003305745280000171
聚酯用作粘合剂膜。
实例3
通过等压方法的具有未增强热塑性皮的板
组装类似于实例2中所述那些的两个夹层板，并使其通过双带连续机器，该机器具有两条相对的环形不锈钢带和8延米的加热加工区。该机器遍及8延米的整个加热加工区和随后的冷却施加两(2)巴的绝对压力。
通过将加热温度设置在205℃并且使用1.5m/min的线速度制造第一个板。通过将加热温度设置在230℃并且使用0.5m/min的线速度制造第二个板。
所得的固结板示出在泡沫芯与PPSU皮层之间的良好的结合线。
根据EN 2243-3，使固结夹层板试样经受爬鼓剥离测试(以25mm/min施加张力)。测试结果示出，在205℃和1.5m/min线速度下制造的夹层的平均剥离强度是250N/75mm，并且在230℃和0.5m/min线速度下制造的夹层的平均剥离强度是260N/75mm。这些剥离强度值明显大于实例1的对照夹层板获得的值。
实例4
具有热固性皮的板
组装夹层板，使其具有
Figure BDA0003305745280000181
泡沫芯(12mm厚)、两个热固性皮以及每个热固性皮与泡沫芯之间的100μm的PSU树脂膜。每个热固性皮在每侧具有2层MTM348FR-7781-38％RC；MTM348FR-7781-38％RC是由索尔维公司(Solvay)提供的预浸料，具有按重量计38％树脂含量，含有MTM348FR阻燃环氧树脂体系和7781E-玻璃织物。
使所组装的夹层板通过实例1的双带连续机器，其中将加热温度设置在175℃，并且使用0.5m/min的线速度。所述温度和时间提供了热固性皮的完全固化。
所得的固化夹层板示出在热固性皮与热塑性膜粘合剂之间的良好的结合线以及在热塑性膜粘合剂与泡沫芯之间的良好的结合。
根据EN 2243-3，使固结夹层板试样经受爬鼓剥离测试(以25mm/min施加张力)。测试结果示出314N/75mm的平均剥离强度。
实例5
通过等容方法的具有玻璃织物增强热塑性皮的夹层板
由
Figure BDA0003305745280000191
泡沫芯(12mm厚)、两个纤维增强热塑性皮、以及每个热塑性皮与泡沫芯之间的100μm的PSU粘合剂膜组装夹层板。通过将连续7781e-玻璃织物压入连续PPSU聚合物膜层使得将织物嵌入聚合物层中，制造出作为连续片材的每个热塑性皮。每个热塑性皮具有按重量计约40％的聚合物含量。
实例1中披露的双带连续机器用于固结夹层板。将加热温度设置在250℃，线速度是1m/min，并且相对的环形带之间的距离是12.5mm。
所得的固结板示出了在纤维增强热塑性皮与粘合剂膜之间的良好的结合线，以及在粘合剂膜与泡沫芯之间的良好的结合。
根据EN 2243-3，使固结夹层板试样经受爬鼓剥离测试(以25mm/min施加张力)。测试结果示出408N/75mm的平均剥离强度。
实例6
通过等容方法的具有玻璃织物增强热塑性皮的夹层
组装了与实例5中的夹层板类似的夹层板，但是通过使所组装的夹层板通过配备有辊毯模块(RCM)的机器进行固结，以遍及材料的所有长度和宽度控制泡沫和夹层的厚度。250℃的温度用于同时获得良好玻璃织物浸渍和PPSU基皮与相邻PSU粘合剂膜的粘附。
根据EN 2243-3，使固结夹层板试样经受爬鼓剥离测试(以25mm/min施加张力)。测试结果示出360N/75mm的平均剥离强度。

Claims (28)

1.一种夹层结构，其包括：
具有两个相反表面的热塑性泡沫芯，
在该热塑性泡沫芯的这些相反表面的至少一个上的热塑性粘合剂膜；
粘附到该热塑性粘合剂膜上的第一复合层，
其中
该第一复合层包含嵌入聚合物或树脂基质中的增强纤维，
该热塑性泡沫芯由具有如通过差示扫描量热法(DSC)以5℃/min的加热速率确定的210℃至240℃的玻璃化转变温度(Tg)的发泡热塑性材料形成，并且所述发泡热塑性材料由包含一种或多种聚(芳基醚砜)(PAES)聚合物的可发泡组合物形成，并且
该热塑性粘合剂膜由聚合物组合物形成，基于该聚合物组合物的总重量，该聚合物组合物包含至少80wt.％的一种或多种聚砜，所述一种或多种聚砜具有如通过DSC以5℃/min的加热速率确定的比该发泡热塑性材料的Tg低至少20℃，优选地为180℃至190℃的Tg。
2.根据权利要求1所述的夹层结构，其中，该发泡热塑性材料由可发泡组合物形成，基于该组合物的总重量，该可发泡组合物包含至少80wt.％的PPSU聚合物，所述PPSU聚合物包含至少50mol.％的具有下式(L)的重复单元(RPPSU)，该mol.％是基于该聚合物中的总摩尔数：
Figure FDA0003305745270000011
优选地，所述PPSU聚合物具有如通过凝胶渗透色谱法(GPC)确定的在30,000至90,000g/mol范围内、包括从40,000至80,000g/mol或从50,000至70,000g/mol的重均分子量(Mw)。
3.根据权利要求1或2所述的夹层结构，其中，该热塑性粘合剂膜的该聚合物组合物中的该聚砜(PSU)具有至少50mol.％的具有下式(U)的重复单元(RPSU)：
Figure FDA0003305745270000021
该mol.％是基于该聚合物中的重复单元的总摩尔数，优选地，该PSU具有如通过凝胶渗透色谱法(GPC)确定的在30,000至110,000g/mol范围内、优选地从40,000至100,000g/mol或50,000至90,000g/mol的重均分子量(Mw)。
4.根据权利要求1至3中任一项所述的夹层结构，其中，该第一复合层包含嵌入热塑性聚合物基质中的增强纤维，该热塑性聚合物基质包含一种或多种热塑性聚合物，优选地，该一种或多种热塑性聚合物选自：聚醚砜(PES)、聚醚醚砜(PEES)、聚苯砜、聚苯硫醚(PPS)、聚砜、聚(芳基醚砜)聚合物、聚苯砜(PPSU)、聚酯、聚酰亚胺、聚醚酰亚胺(PEI)、聚醚酮酮(PEKK)、聚醚醚酮(PEEK)、聚芳基醚酮(PAEK)聚合物、聚醚酮酮(PEKK)、聚酮、聚酰胺、聚邻苯二甲酰胺、聚甲基丙烯酸酯、聚氨酯、聚芳基醚、聚芳基硫化物、聚亚苯基、聚苯醚(PPO)、及其共聚物。
5.根据权利要求1至3中任一项所述的夹层结构，其中，该第一复合层包含嵌入可固化树脂基质中的增强纤维，该可固化树脂基质包含一种或多种环氧树脂和至少一种固化剂。
6.根据前述权利要求中任一项所述的夹层结构，其中，该第一复合层中的这些增强纤维呈连续单向纤维、短切纤维、织造织物、或随机布置的纤维的非织造垫或面纱的形式。
7.根据前述权利要求中任一项所述的夹层结构，其中，该第一复合层中的这些增强纤维选自：碳纤维，玻璃纤维，聚合物纤维，由碳化硅、氧化铝、硼、或石英形成的纤维，及其组合。
8.根据前述权利要求中任一项所述的夹层结构，其进一步包括在该第一复合层上的一个或多个附加的复合层，每个附加的复合层包含嵌入聚合物或树脂基质中的增强纤维。
9.根据前述权利要求中任一项所述的夹层结构，其中，该热塑性泡沫芯没有任何增强纤维、或者任何延伸穿过其厚度的孔。
10.根据前述权利要求中任一项所述的夹层结构，其中，该泡沫芯具有如通过ASTMD1622测量的在45Kg/m3至150Kg/m3范围内的密度。
11.根据前述权利要求中任一项所述的夹层结构，其中，该泡沫芯具有在3mm至30mm范围内的厚度，并且该粘合剂膜具有在25至250微米(μm)范围内的面积重量。
12.根据前述权利要求中任一项所述的夹层结构，其中，该第一复合层具有在200至2000gsm范围内，在一些实施例中，450至600gsm的面积重量。
13.一种用于制造夹层结构的连续方法，所述方法包括：
(a)形成至少具有以下部件的多层组件：具有两个相反表面的热塑性泡沫芯；在该热塑性泡沫芯的这些相反表面的一个或两个上的热塑性粘合剂膜；在该/每个热塑性粘合剂膜上的纤维增强复合材料的一个或多个层，其中该热塑性泡沫芯由具有至少200℃、优选210℃至240℃的玻璃化转变温度(Tg)的发泡热塑性材料形成，并且该/每个热塑性粘合剂膜由热塑性聚合物组合物形成，该热塑性聚合物组合物包含一种或多种聚砜(PSU)，该一种或多种聚砜具有的Tg比该发泡热塑性材料的Tg低至少20℃，其中Tg是通过差示扫描量热法(DSC)以5℃/min的加热速率确定的；
(b)使该多层组件在双带压机的两条环形带之间通过；以及
(e)在该夹层结构通过该双带压机期间将其加热至从200℃至260℃的温度持续1至10分钟的时间段。
14.根据权利要求13所述的方法，其中，步骤(b)以0.5至5m/min的线速度、在通过这些环形带施加的小于5巴、优选1至2巴的正压力下进行。
15.根据权利要求13所述的方法，其中，步骤(b)以0.5至5m/min的线速度进行，并且这些环形带之间的距离在从3mm至40mm的范围内，并且其中，这些环形带之间的所述距离比该多层组件在(a)时的总厚度小1mm至10mm。
16.根据权利要求13至15中任一项所述的方法，其中，该发泡热塑性材料由包含一种或多种聚(芳基醚砜)(PAES)聚合物的可发泡组合物形成。
17.根据权利要求13至16中任一项所述的方法，其中，该发泡热塑性材料由可发泡组合物形成，基于该组合物的总重量，该可发泡组合物包含至少80wt.％的PPSU聚合物，所述PPSU聚合物包含至少50mol.％的具有下式(L)的重复单元(RPPSU)，该mol.％是基于该聚合物中的总摩尔数：
Figure FDA0003305745270000041
优选地，该PPSU聚合物具有如通过凝胶渗透色谱法(GPC)确定的在30,000至90,000g/mol范围内、可选地从40,000至80,000g/mol或从50,000至70,000g/mol的重均分子量(Mw)。
18.根据权利要求13至17中任一项所述的方法，其中，该热塑性粘合剂膜的该组合物中的该PSU具有如通过DSC以5℃/min的加热速率确定的小于200℃、优选180℃-190℃的Tg。
19.根据权利要求18所述的方法，其中，该热塑性粘合剂膜的该组合物中的该PSU具有至少50mol.％的具有下式(U)的重复单元(RPSU)：
Figure FDA0003305745270000042
该mol.％是基于该聚合物中的重复单元的总摩尔数，优选地，该PSU具有如通过凝胶渗透色谱法(GPC)确定的在30,000至110,000g/mol范围内、可选地从40,000至100,000g/mol或从50,000至90,000g/mol的重均分子量(Mw)。
20.根据权利要求13至19中任一项所述的方法，其中，该纤维增强复合材料包含嵌入热塑性聚合物基质中的增强纤维，该热塑性聚合物基质包含具有如通过DSC以5℃/min的加热速率确定的在210℃至240℃范围内的Tg的无定形热塑性材料。
21.根据权利要求13至19中任一项所述的方法，其中，该纤维增强复合材料包含嵌入热塑性聚合物基质中的增强纤维，该热塑性聚合物基质包含选自以下的一种或多种热塑性聚合物：聚醚砜(PES)、聚醚醚砜(PEES)、聚苯砜、聚苯硫醚(PPS)、聚砜、聚(芳基醚砜)聚合物、聚苯砜(PPSU)、聚酯、聚酰亚胺、聚醚酰亚胺(PEI)、聚醚酮酮(PEKK)、聚醚醚酮(PEEK)、聚芳基醚酮(PAEK)聚合物、聚醚酮酮(PEKK)、聚酮、聚酰胺、聚邻苯二甲酰胺、聚甲基丙烯酸酯、聚氨酯、聚芳基醚、聚芳基硫化物、聚亚苯基、聚苯醚(PPO)、及其共聚物。
22.根据权利要求13至19中任一项所述的方法，其中，该纤维增强复合材料包含嵌入可固化树脂基质中的增强纤维，该可固化树脂基质包含一种或多种环氧树脂和至少一种固化剂。
23.根据权利要求20至22中任一项所述的方法，其中，这些增强纤维选自：碳纤维，玻璃纤维，聚合物纤维，由碳化硅、氧化铝、硼、石英形成的纤维，及其组合。
24.根据权利要求13至23中任一项所述的方法，其中，该泡沫芯具有如通过ASTM D1622测量的在45Kg/m3至150Kg/m3范围内的密度。
25.根据权利要求13至24中任一项所述的方法，其中，该泡沫芯具有在3mm至30mm的范围内的厚度。
26.根据权利要求13至25中任一项所述的方法，其中，该/每个粘合剂膜具有在25至250微米(μm)范围内的面积重量。
27.根据权利要求13至26中任一项所述的方法，其中，该/每个纤维增强复合材料层具有在200至2000gsm范围内，在一些实施例中，450至600gsm的面积重量。
28.根据权利要求13至27中任一项所述的方法，其中，这些环形带由弹性材料或不锈钢制成。
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