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CN102307919A - 包含聚醚酮酮结系层的组件 - Google Patents

包含聚醚酮酮结系层的组件 Download PDF

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CN102307919A
CN102307919A CN2010800070201A CN201080007020A CN102307919A CN 102307919 A CN102307919 A CN 102307919A CN 2010800070201 A CN2010800070201 A CN 2010800070201A CN 201080007020 A CN201080007020 A CN 201080007020A CN 102307919 A CN102307919 A CN 102307919A
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Prior art keywords
substrate
tie layers
assembly
pekk
amorphous
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C·A·伯蒂罗
G·S·欧布莱恩
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Arkema Inc
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Arkema Inc
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Priority to CN201510859570.0A priority Critical patent/CN105295025A/zh
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Abstract

使用由无定形聚醚酮酮构成的结系层来连接多个基片以形成叠层材料以及其他组件。

Description

包含聚醚酮酮结系层的组件
发明领域
本发明涉及无定形聚醚酮酮在诸如复合材料、叠层材料以及类似物的组件中作为结系层的用途。
相关技术的讨论
在近几十年，在设计包含多个不同材料层的叠层材料、复合材料以及其他组件中已经投入了相当大的开发努力。对于许多最终用途应用，使用单一材料来制造所希望的部件是不可行的，这是由于任何已知的材料都不能满足特定的多重性能要求。例如，可能需要一个部件同时在强度和刚度方面很高并且是耐压力的、耐溶剂/化学物的、并且在高温下是尺寸稳定的。然而，在可能需要在复合材料或叠层材料中使用的多个相异层之间直接实现令人满意的粘附或结合常常被证明是具有挑战性的。复合材料层之间差的相容性会限制此类组件所展现出的特性。具体地，某些热塑性塑料(特别是结晶的和/或高温热塑性塑料)展现出了与其他材料的差的粘附，这已经归因于此类热塑性塑料不能充分地“润湿”相异物质的表面，从而当该复合材料被用于高要求的环境中时导致了与层离和结构整体性丧失相关的问题。因此，有利的是开发用于组装复合材料、叠层材料以及类似物的改进的方法，这些方法通过确保复合材料或叠层材料层之间的良好结合而避免了此类困难。
发明简述
本发明提供了一种组件，该组件包括一个第一基片以及一个第二基片，其中一个由无定形聚醚酮酮构成的结系层被置于所述第一基片与所述第二基片之间并且与它们相接触。此类组件可以按如下方法来制备：将一个基片用无定形聚醚酮酮涂覆，并且然后通过将这些基片压在一起同时加热该聚醚酮酮结系层来将另一个基片与该涂覆的基片进行连接。替代性地，可以采用一种共挤出工艺。在一个基片包括一种结晶的和/或高温热塑性塑料如一种结晶的聚(芳醚酮)、而这种热塑性塑料在缺少该结系层时没有展现出完全令人满意的对另一个基片表面的粘附性的情况下，本发明是尤其有用的。
附图简要说明
图1示出了用PEKK和PEEK上胶的纤维的显微图像、并且显示了各种胶料在纤维中的失效模式。
本发明的某些实施方案的详细说明
根据本发明的组件有利地是使用由无定形聚醚酮酮构成的结系层来制造的。适合用于本发明中的无定形聚醚酮酮包含(并且优选地基本上由其组成或者由其组成)由以下化学式I和II所代表的重复单元：
-A-C(＝O)-B-C(＝O)-  I
-A-C(＝O)-D-C(＝O)-  II
其中，A是一个p，p’-Ph-O-Ph-基团，Ph是一个亚苯基，B是对-亚苯基，并且D是间-亚苯基。改变该聚醚酮酮中的化学式I∶化学式II(T∶I)的异构体之比以提供一种无定形(非晶态)的聚合物。对于本发明的目的，无定形聚合物是指通过差示扫描热量法(DSC)并没有展现出结晶性熔点的一种聚合物。
聚醚酮酮是本领域中所熟知的，并且可以使用任何适当的聚合技术来制备，这些技术包括在以下专利(为所有目的通过引用各自以其整体结合在此)中所描述的方法：美国专利号3,065,205；3,441,538；3,442,857；3,516,966；4,704,448；4,816,556；以及6,177,518。可以采用多种聚醚酮酮的混合物。
具体地说，可以通过改变用于制备聚醚酮酮的不同单体的相对量值而如所希望地调节化学式I∶化学式II之比(在本领域中有时称为T/I之比)。例如，可以通过使对苯二酰氯和间苯二酰氯的混合物与二苯醚进行反应来合成一种聚醚酮酮。增大对苯二酰氯相对于间苯二酰氯的量值将增大化学式I∶化学式II(T/I)之比。总而言之，具有较高的化学式I∶化学式II之比的聚醚酮酮与具有较低的化学式I∶化学式II之比的聚醚酮酮相比是更加结晶化的。具有的T/I之比为从约55∶45至约65∶35的一种无定形聚醚酮酮特别适合用于本发明中。
适合的无定形聚醚酮酮可以从商业来源获得，例如像由OxfordPerformance Materials，Enfield，Connecticut在商品名OXPEKK下所销售的某些聚醚酮酮类，包括OXPEKK-SP聚醚酮酮。
用于形成该结系层的聚合物组合物可以另外地由除了无定形聚醚酮酮之外的组分组成，例如稳定剂、颜料、加工助剂、填充剂、以及类似物。在本发明的某些实施方案中，该聚合物组合物主要由或由无定形聚醚酮酮组成。例如，该聚合物组合物可以不含有或基本上不含有除无定形聚醚酮酮之外的任何类型的聚合物。
本发明对于多层结构是有用的，例如像薄膜、片材、管道以及空心体如储存罐，其中使用一个由无定形聚醚酮酮构成的结系层来将一个第一基片层粘附到一个第二基片层上。因此该多层结构可以包括一个结系层(T)、直接附连于结系层(T)的一个第一面(表面)上的一个第一基片层(S1)、以及直接附连于结系层(T)的一个第二面(表面)上的一个第二基片层(S2)，这样使得该结系层(T)被夹在第一基片层(S1)与第二基片层(S2)之间。当然，在该组件中可以存在附加的层和部件，包括被置于其他基片层之间的一个或多个另外的结系层。
通过该结系层相连接的这些基片层之一或二者可以例如是一个片材或一个薄膜。这些基片可以包括任何适当的材料，例如像金属、塑料(热塑性的或热固性的)、陶瓷、或玻璃。该基片可以是一种复合材料，例如像玻璃纤维增强的塑料。该薄膜或片材的厚度可以适当地进行选择并且可以是例如从约0.01至约10mm。
在一个实施方案中，该第一基片或第二基片中的至少一个包括一种结晶的(包括半结晶的)和/或高温热塑性塑料，因为这些材料通常展现出不完全令人满意的、对不同类型的基片表面的界面粘附性。根据本发明的无定形聚醚酮酮的结系层有助于改善此种粘附性，由此增强所得组件的机械特性和其他特性。适当的结晶的和/或高温热塑性塑料包括但不限于：聚芳醚酮(如结晶的聚醚酮(PEK)、结晶的聚醚醚酮(PEEK)、结晶的聚醚酮酮(PEKK)、聚醚醚醚酮(PEEEK)、聚醚醚酮酮(PEEKK)、聚醚酮醚醚酮(PEKEKK)、以及聚醚酮酮酮(PEKKK))、聚酰亚胺、聚醚酰亚胺、聚酰胺酰亚胺、聚砜、聚醚砜、聚芳基醚、聚碳酸酯、液晶聚合物、聚苯硫醚、聚亚芳基(聚亚苯基)、聚酰胺、聚邻苯二甲酰胺、聚芳族酯、以及类似物。
在另一个实施方案中，该第一基片或第二基片中至少一个是金属的，例如一个金属片、箔片或类似物。该基片可以包括任何适当的金属或金属合金，如钢、铝、铝合金、铜、金、银或类似物。
该结系层典型地是相对薄的，例如从约1至约100微米厚。在本发明的一个实施方案中，该第一与第二基片表面之间的界面被该结系层完全填充或覆盖，但在其他实施方案中该结系层可以是不连续的。
在一个实施方案中，本发明的组件是通过对已知的共挤出方法进行调整而制造的，特别是其中通过该结系层相连接的这两个基片层均是基于热塑性聚合物。例如，用于制造此类组件的装置可以是普遍用于热塑性聚合物的共挤出的、任何常规的或标准的挤出机、模口或流分配器(stream distributors)。各个聚合物层的厚度将取决于对各个挤出机的流速的调节。一般，模口和挤出机的温度应当基于有待在该结系层和这些基片层中使用的聚合物的特征和特性来进行选择，这样使得这些材料能够被挤出。
本发明的组件可以被挤出为任何常规的形式，包括薄膜、板、片材、管道、或通过共挤出而是常规地可获得的任何其他形状。
压缩模制、间歇的匹配模口固结(intermittent matched dieconsolidation)、双带压机固结、复合辊成型、传递模制、以及其他此类技术也可以与本发明相关联地使用。例如，该组件可以通过以下方法制备：将在组成上对应于所希望的结系层的一个片材或薄膜放置在一个第一基片与一个第二基片之间，并且在对于充分软化这些层中的至少一个而言是有效的温度下加热所得的“夹层”以使它能流动并且与一个相邻层进行紧密接触，由此在冷却该组件时形成一种粘性结合。典型地，将希望的是在该“夹层”上施加压力从而增强在结系层与这些基片层之间达到的粘附程度。可以进行该组件的热压成型从而获得一种特别希望的形状或轮廓。
在又一个实施方案中，该组件可以通过首先将一个根据本发明的结系层粘附到一个第一基片上来形成。这可以例如通过将该结系层与该第一基片共挤出、或者通过将一片结系层与一片第一基片压在一起同时加热、或者通过将该结系层挤出到该第一基片上而完成。然后可以将所得的结系层/第一基片的子组件连接到一个第二基片上，其方式为将该第二基片与结系层的另一侧进行接触，同时施加足够的热和压力从而在结系层与第二基片的表面之间创造所希望程度的粘附。也可以采用包覆模制或挤出模制的技术。例如，可以将该结系层/第一基片的子组件定位在一个模具中并将一种加热过的聚合物组合物(对应于所希望的第二基片的组成)引入该模具中，使得它与结系层的可用的表面的至少一部分相接触。若希望的话，可以对包覆模制的条件进行选择，使得该结系层/第一基片的子组件在此种包覆模制的过程中经历形状上的改变(例如，该子组件可以被热压成形)。替代性地，可以将该加热过的聚合物组合物作为一个涂层而挤出模制到结系层表面上以形成该第二基片层。
在又一个实施方案中，可以将该结系层的熔体挤出在第一与第二基片层的预成型的片材之间。这可以恰在这两个片材的层叠之前进行。
该结系层还可以通过将无定形聚醚酮酮的溶液施加到一个基片表面并接着去除溶剂而形成。用于无定形聚醚酮酮的适当溶剂是本领域已知的并且包括例如：卤代烃类(特别是氯代烃类，如邻-二氯苯、1，2，4-三氯苯、二氯甲烷和四氯乙烯)、硝基苯、以及水性无机酸(例如硫酸和/或硝酸)。该溶剂可以通过任何适当的方法如加热和/或施加真空来从该被涂覆的基片上去除。
根据本发明制备的组件可以用于在其中常规地采用或已提出要采用此类叠层材料或复合材料的任何最终用途应用中。代表性的应用包括用于航空/飞行器、汽车和其他车辆、船只、机械装置、重型设备、储存罐、管道、运动设备、工具、生物医学器件(包括待植入人体中的器件)、建筑物部件、风机叶片以及类似物的复合材料和叠层材料(包括二维和三维的面板和片材)。与未使用基于无定形聚醚酮酮的结系层而制备的组件相比，在此描述的本发明的益处包括更高的拉伸强度、更高的抗压强度、更高的剥离强度、增强的对溶剂和化学物及水的耐受性、以及改进的抗层离性。
实例
实例1.生产PEKK薄膜：通过在一台装配有12英寸薄膜模口的1英寸Davis Standard挤出机上对无定形聚醚酮酮A-PEKK(来自Oxford Performancematerials，T/I之比为60/40)球粒进行熔体加工来生产一个A-PEKK薄膜。将聚合物以较低的螺杆速度(20-80RPM)并在315℃-325℃下进行加工。该挤出机装配有一个来自Davis Standard的标准流延膜取下架(standard castfilm take off stack)，在150℃下运行。
生产T/I之比为70/30或更高的、结晶等级的薄膜也是有可能的但是更加困难。这些薄膜的快速冷却和结晶要求更高的挤出机温度和熔体温度(365℃-375℃)以及更高的用于该取下设备的温度(220℃-250℃或更高)。
实例2.使用PEKK作为结系层来生产并测试叠层材料：试验样品由1英寸乘5英寸的金属或玻璃条(见表1)以及1英寸乘1英寸乘0.7英寸的、通过在实例1中所描述的方法而形成的PEKK片材组成。将这些试验样品的表面用丙酮清洁以在模制之前去除任何润滑脂或油。使用一台Carver压机以及两个12英寸乘12英寸的、带有用于夹持试验样品的小的1英寸乘5英寸压痕的铝块来对这些样品进行压缩模制。将该压机模具预加热至220℃-230℃(对于A-PEKK片材)或260℃-290℃(对于晶态PEKK)。在预加热之后，从压机中取出模具并将试验片材和1英寸乘1英寸的PEKK片材仔细组装成一个3层结构，以便不污染这些结合表面。这种构造的组成为，一个PEKK片材位于适当的试验材料的两个片材之间。接着将该模具再组装并且放回到压机中并且再加热到该试验温度持续约1分钟。然后将这些组件在2000psi下压制5分钟，并接着取出并允许其在测试结合强度之前在室温下于50％的相对湿度下保持至少24小时。
使用Zwick-Roell Z050拉伸试验在一台仪器中评估结合强度，使用一种与ASTM D3528-96(2008)“Standard Test Method For Strength PropertiesOf Double Lap Shear Adhesive Joints By Tension Loading(用拉力负荷法测定双搭接剪切粘结接头的强度特性的标准试验方法)”相类似的方法，其中十字头速度为1.27mm/min。结果呈现在下表1和表2中。
表1
使用PEKK作为粘合剂的、相似基片的搭接剪切试验
Figure BPA00001417896400061
Figure BPA00001417896400071
表2
使用PEKK作为粘合剂的、对于相似和相异基片的搭接剪切试验
Figure BPA00001417896400072
Figure BPA00001417896400081
对与其他相似的高温聚合物相比PEKK所提供的改进的粘附性的说明
聚醚醚酮是具有与PEKK相似的结构以及使用温度的一种聚合物，但它是用不具有间苯二甲酸酯(即T/I＝100)的纯的对式结构生产的。该图的显微照片展示了，PEEK具有差得多的对玻璃纤维的粘附性，因为这些纤维在被冷冻断裂(cryrofractured)时似乎从基质中拉离，而用PEKK制成的样品的显微照片显示，这些纤维并没有拉出并且PEKK仍附连于这些纤维上。如该图展示的，该PEKK复合材料中的失效是内聚性的，因为这种失效是在PEKK基质中。在此情况下的断裂面显示了由于纤维与PEKK基质之间的有效负荷转移而产生的显著的延展性。相比之下，PEEK系统中的失效是粘性的，因为这些纤维彻底从基质中被拉出。这个断裂的表面显示了一个完全脆性断裂的过程，这表明在此情况下纤维与基质之间的相互作用是欠有效的。在此系统中不预期负荷转移是有效的。通过内聚性失效产生的、破坏一个件的能量依赖于该基质本身的强度并且一般被认为是高于粘性失效。

Claims (10)

1.一种组件，包括一个第一基片以及一个第二基片，其中一个由无定形聚醚酮酮构成的结系层被置于所述第一基片与所述第二基片之间并且与它们相接触。
2.如权利要求1所述的组件，其中所述第一基片具有一个与所述结系层相接触的表面，该表面由玻璃、塑料、陶瓷、和/或金属构成。
3.如权利要求1所述的组件，其中所述第二基片具有一个与所述结系层相接触的表面，该表面由一种结晶的和/或高温热塑性塑料构成。
4.如权利要求1所述的组件，其中所述第一基片是金属的并且所述第二基片由一种结晶的和/或高温热塑性塑料构成。
5.如权利要求1所述的组件，其中所述结系层是从约1至约100微米厚。
6.如权利要求1所述的组件，其中该无定形聚醚酮酮包括由以下化学式I和II所代表的重复单元：
-A-C(＝O)-B-C(＝O)- I
-A-C(＝O)-D-C(＝O)- II
其中，A是一个p，p’-Ph-O-Ph-基团，Ph是一个亚苯基，B是对-亚苯基，并且D是间-亚苯基。
7.如权利要求1所述的组件，其中该无定形聚醚酮酮具有从约65∶35至约55∶45的T∶I比率。
8.如权利要求1所述的组件，其中所述第一基片和所述第二基片是处于片材的形式。
9.如权利要求1所述的组件，其中所述第二基片具有一个与所述结系层相接触的表面，该表面由一种选自下组的结晶的聚(芳醚酮)构成，该组由以下各项组成：PEK、PEEK、PEEEK、PEEKK、PEKEKK以及PEKKK。
10.一种用于制造组件的方法，所述方法包括使用一个由无定形聚醚酮酮构成的结系层将一个第一基片连接到一个第二基片上。
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