CN108780675A - 固体绝缘材料、其用途和由其制造的绝缘体系 - Google Patents

固体绝缘材料、其用途和由其制造的绝缘体系 Download PDF

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CN108780675A
CN108780675A CN201780016081.6A CN201780016081A CN108780675A CN 108780675 A CN108780675 A CN 108780675A CN 201780016081 A CN201780016081 A CN 201780016081A CN 108780675 A CN108780675 A CN 108780675A
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insulating materials
compound
curing catalysts
insulating material
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CN108780675B (zh
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J.休伯
D.希尔姆
M.于布勒
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Siemens AG
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Abstract

本发明涉及固体绝缘材料、特别地带形式的固体绝缘材料、其在真空浸渍工艺中的用途和由其制造的绝缘体系以及具有该绝缘体系的电机，特别地用于中压和高压范围，即用于中压和高压机器，尤其是在中压和高压范围内的旋转电机以及用于电气开关装置的半成品。所述固体绝缘材料和由其制造的绝缘体系的特征在于，它可以无酸酐的方式制备，其中固化催化剂是1H‑咪唑和/或1H‑咪唑衍生物与含环氧乙烷基团的化合物的加合物。

Description

固体绝缘材料、其用途和由其制造的绝缘体系
本发明涉及固体绝缘材料、特别地带形式(带状)的固体绝缘材料、其在真空浸渍工艺中的用途和由其制造的绝缘体系以及具有该绝缘体系的电机，特别地用于中压和高压范围，即用于中压和高压机器、尤其是在中压和高压范围内的旋转电机以及用于电气开关装置的半成品。
电机(电动机、发电机)在其定子叠片铁芯的大部分纵向槽中具有通常由铜或其它高导电性材料制成的特定类型的线圈绕组或导体棒
在电动机的情况下，通过以时间选择性的方式提供电流(通电)产生沿所有方向传播的磁场，其驱动悬挂在定子的孔中的并且自由旋转的转子，所述转子例如由于多个施加的永磁体而以强制旋转的形式对感应磁场作出反应，并因此将电能转换为动能。在此，叠片铁芯电接地，而线圈却处于高的千伏电位。装配在定子槽中的线圈因此必须相对于地电位电绝缘。为此，每一个线圈例如用特定的带例如云母带多次(重复)地且以限定重叠的方式(definiert-überlappt)绝缘。
优选使用云母，因为其作为颗粒形式的、特别地作为片状的无机阻挡材料能够在局部放电下有效且长时间地，例如在机器的整个寿命期间延缓电蚀，并且具有良好的化学稳定性和耐热性。云母带由云母纸和一种或多种载体如织物、膜(箔)组成，其通过胶带粘合剂(Bandkleber)相互连接。云母带是必要的，因为云母纸单独地不具有绝缘过程所需的机械强度。根据应用，可将添加剂添加到胶带粘合剂中，例如固化催化剂，其对外部施加的浸渍剂的热固化具有引发作用：在用云母带绝缘的线圈被装配到定子叠片铁芯中并电接通之后，为了避免在后续的操作中的局部放电而消除绕组空腔中和特别地定子叠片铁芯的槽间隙中的空气。由于从通电的经绝缘的线圈到叠片铁芯的距离通常保持尽可能小，因而在那里几kV/mm的场强并不罕见。相应地，绝缘材料经受应力。
作为根据现有技术的浸渍剂，已经发现热可固化的环氧树脂/酸酐混合物适用于真空浸渍工艺。
它们用于浸渍由其各个部件组成的具有装配好的且经云母带绝缘的线圈的电机定子或用于单独地浸渍线圈或导体棒。
在特定的真空浸渍工艺(VPI(真空压力浸渍)工艺)的过程中，这些定子或线圈迄今都是在真空室中整个用低粘度的环氧树脂/邻苯二甲酸酐配制物充满，并且随后在加压下浸渍。通常在工业炉中在标准压力下进行最终固化。在此，固化催化剂具有如下的功能：使通常由环氧树脂和邻苯二甲酸酐组成的低粘度的浸渍剂在给定的温度下在特定时间内凝胶化。迄今为止，工业标准浸渍剂是经蒸馏的双酚A-二缩水甘油醚和甲基六氢邻苯二甲酸酐的混合物。这种混合物具有足够低的粘度，从而一方面确保带绝缘的完全浸渍以及另一方面在不存在固化催化剂的情况下确保足够的储存稳定性。固化催化剂通常至少也被包含在固体绝缘材料如云母带中。这种云母带通过胶带粘合剂被保持在一起，因此必要的是，胶带粘合剂和固化催化剂相对于彼此是惰性的。
尤其有利的情形是，所有三种组分，即胶带粘合剂、固化催化剂和所施加的浸渍剂在VPI工艺期间只在相遇时才彼此反应。如此实现了所述绝缘的最佳的交联和连接、相容性以及缩孔自由度(Lunkerfreiheit)，这又导致在固化过程中随后形成的电机的“主绝缘”的优化的寿命。
由于对邻苯二甲酸酐的无限制使用的毒理学担忧，将来会使用不含邻苯二甲酸酐或完全无酸酐(或不含酸酐)的基于环氧化物的浸渍剂，其在使用固化催化剂的情况下聚合。
新型的固化催化剂与不含酸酐的浸渍剂相匹配。越来越多地使用不含酸酐的浸渍剂，如从较早的申请DE 102015214872.6和DE 102015213534.9中所知的，其公开内容在此并入本说明书中。
这些提出了一方面使用咪唑和/或吡唑及其衍生物作为固化催化剂，另一方面提出共价桥连的二咪唑衍生物和/或共价桥连的二吡唑衍生物作为固化催化剂，其例如为缩合产物和/或加合(加成)产物。这些是固体绝缘材料中的固化催化剂，由于分子扩大和在原来亲电子中心处的可能的额外相互作用，其具有比简单(烷基)咪唑更低的挥发性。尽管挥发性较低，但与简单的(烷基)咪唑相比，相对于基于环氧树脂的不含酸酐的浸渍树脂的反应性不受或仅受到可忽略的不利影响。因此，这些体系代表了基于环氧树脂的不含酸酐的浸渍树脂的优异的固化催化剂。
尽管如此，仍然需要新型的用于不含酸酐的缩水甘油醚环氧树脂和缩水甘油酯环氧树脂的固化催化剂，特别是需要与现有技术中已知的咪唑、二咪唑、吡唑和/或二吡唑相比可以适于大规模生产的方式由易得的原料制备和/或具有与环氧树脂更好的化学相容性的那些。
因此，本发明的目的在于提供一种具有固化催化剂的固体绝缘材料，其克服现有技术的缺点。此外，本发明的目的还在于提供固体绝缘材料在真空浸渍工艺中的用途并最终提供具有以这种方式制造的绝缘系统的电机，其中通常避免使用呼吸道致敏化的邻苯二甲酸酐或有机酸酐。
该目的通过如在说明书、实施例和权利要求中公开的本发明的主题来实现。
因此，本发明的主题是一种固体绝缘材料，它可与不含酸酐的浸渍剂一起用于以真空浸渍工艺制造绝缘体系，其中所述固体绝缘材料包括载体、阻挡材料、固化催化剂和胶带粘合剂，所述固化催化剂和胶带粘合剂相对于彼此呈惰性，但在真空浸渍条件下与不含酸酐的浸渍剂在浸渍温度下以1小时至15小时的凝胶化时间反应，其中固化催化剂可通过至少一种1H-咪唑和/或1H-咪唑衍生物与包含环氧乙烷基团的化合物反应而获得。
此外，本发明的主题亦为如此制备的绝缘体系在电机、优选地旋转电机、特别优选地在中压和高压范围内的旋转电机中以及在电气开关装置、中压和高压应用、套管、变压器套管、发电机套管和/或套管以及在相应的半成品中的用途。
最后，本发明的主题还有电机、优选地旋转电机、特别优选地在中压和高压范围内的旋转电机以及电气开关装置、中压和高压应用、套管、变压器套管、发电机套管和/或套管、以及相应的半成品，其包括这种类型的绝缘体系。
尽管固化催化剂可通过使1H-咪唑和/或1H-咪唑衍生物中的至少一种与包含环氧乙烷基团的化合物反应来获得，但它也可以根据任意的其它合成途径来制备。固化催化剂例如仅为1H-咪唑和/或1H-咪唑衍生物与包含环氧乙烷基团的化合物的加合物(加成产物)。
根据本发明的有利的实施方式，固化催化剂(例如1H-咪唑和/或1H-咪唑衍生物与包含环氧乙烷基团的化合物的加合物)具有在例如1至15mmol/g(毫摩尔/克)的范围内的氮密度D，特别地D在1·10-3mol/g<D<13·10-3mol/g、优选地2.5·10-3mol/g至10·10-3mol/g以及最优选地4.5·10-3mol/g至9·10-3mol/g的范围内。这里所提及的质量特异性的、能够聚合的摩尔氮密度D由单位10-3mol/g(相当于千分之一摩尔每克)定义，这说明了每分子的具有非芳族和同时非键合的电子对的氮原子的含量。
例如，下列公开了根据现有技术的固化催化剂的化合物
结构I：根据现有技术的常规固化催化剂
的氮密度可如下来确定：代表根据现有技术的常规固化催化剂的所示分子的摩尔质量为M：638.89g/mol。它具有3个能够聚合的氮电子对，由此参比氮密度示例性地为3mol/638.89g＝4.7×10-3mol/g。
在作为1H-咪唑和/或1H-咪唑衍生物与包含环氧乙烷基团的化合物的加合物的固化催化剂的本发明的实施方式中，可在包含粘合剂的云母纸中提供固化催化剂，其可以这样的方式来改性，使得它在50-80℃的温度下变得真空稳定。例如，这种固化催化剂在70℃下的蒸气压小于10-4毫巴，并且还具有合适的动态粘度。
根据本发明的优选实施方式，固化催化剂呈现出在1至10000Pa·s、特别地5至5000Pa·s且特别优选地10至3000Pa·s的范围内的动态粘度。
根据本发明的另一个优选实施方案，固化催化剂在浸渍温度下表现出小于10-1毫巴的蒸气压，特别地在70℃下在10-2毫巴至10-8毫巴、优选地10-3毫巴至10-7毫巴且特别地10-4毫巴至10-6毫巴的范围内。
根据本发明使用并且可通过使至少1H-咪唑和/或1H-咪唑衍生物与包含环氧乙烷基团的化合物反应得到的固化催化剂优选地通过加成反应获得，如下面示意性所示的。
下面将依据表格更详细地描述本发明，该表格示出了用于例如根据反应方程式I和/或II中所示的机理之一制备固化催化剂的可能反应物的概述。
在此，行给出了示例性的包含环氧乙烷基团的反应物以及列给出了示例性的1H-咪唑和/或1H-咪唑衍生物：特别地，列中使用的缩写具有以下含义：
Im：1H-咪唑；
2m-Im：1H-2-甲基咪唑；
2e-Im：1H-2-乙基咪唑；
2e-4m-Im：1H-2-乙基-4-甲基咪唑；
4e-2Ph-Im：1H-4-乙基-2-苯基咪唑，和
3,5m-Pyr：1H-3,5-二甲基吡唑。
给出的数值在各自的情况下对应于固化催化剂(即相应的加合产物)的氮密度D，如上所述。
作为包含环氧乙烷基团的化合物，使用例如缩水甘油醚和/或缩水甘油酯化合物。示例性化合物列于下表中，其中酯衍生物和/或在此示例性地提及的含有环氧乙烷基团的化合物的对于本领域技术人员显而易见的其他衍生物在所有情况下也包括在本发明的范围内。
表1：用于制备固化催化剂的反应物的实例
实施例
三羟甲基丙烷三缩水甘油醚-三-(1H-2-甲基咪唑)加合物的合成
通过滴液漏斗在搅拌下将相对于1H-咪唑衍生物5％摩尔不足的工业级三羟甲基丙烷三缩水甘油醚缓慢滴加到带回流冷凝器的三颈烧瓶中，其中在室温下存在在20ml甲苯中的5g 1H-2-甲基咪唑，并在130℃下回流溶解10分钟。
然后将其回流几小时。随后，能够获得橙色、透明、高粘度的液体，将其在50-100℃下真空干燥。
在70℃下加入蒸馏的双酚A二缩水甘油醚的5％(w/w)混合物以进行凝胶化和阴离子固化。
对于三羟甲基丙烷三缩水甘油醚-三(1H-2-乙基-4-甲基咪唑)加合物、对于新戊基二缩水甘油醚-双(1H-2-乙基-4-甲基咪唑)加合物、对于双酚F二缩水甘油醚-双(1H-2-甲基咪唑)加合物以类似的方式进行，其中蒸馏的双酚F二缩水甘油醚也预先溶解在甲苯中。
作为胶带粘合剂，在1H-咪唑和/或1H-咪唑衍生物与包含环氧乙烷基团的化合物的上述加合物作为固化催化剂存在下，优选地使用如DE102015205328.8中所述的胶带粘合剂，其公开内容在此引入本说明书的主题。
此外，例如，选自以下组的化合物可用于固体绝缘材料：
三氯甲烷二甲醇(CAS号26896-48-0或26160-83-8)，
三羟甲基丙烷(CAS号77-99-6)，
枝状羟基官能聚合物(CAS号326794-48-3或462113-22-0)，
聚己内酯三醇(CAS号37625-56-2)，
聚己内酯四醇(CAS号35484-93-6)。
胶带粘合剂将至少一个载体和阻挡材料连接在固体绝缘材料中。它以1-30重量％、优选地2-15重量％、特别优选地5-10重量％的量存在于固体绝缘材料中。
载体以织造织物例如玻璃纤维织造织物、非织造织物(“无纺布”)例如羊毛织物、特别地聚酯羊毛织物，纸和/或膜(箔)的形式存在于固体绝缘材料中。在这种情况下，膜形式的载体也可被穿孔。
在固体绝缘材料中，优选地颗粒状的阻挡材料位于该载体处、之中和/或之上。
阻挡材料优选地至少部分地呈片状。更具体地，例如可使用云母作为阻挡材料。
根据优选的实施方式，使用涂覆的颗粒形式的阻挡材料。这特别地可为金属氧化物涂覆的颗粒形式的阻挡材料，例如氧化锡、氧化锌或氧化钛涂覆的颗粒。
在此，根据进一步的实施方式提供颗粒形式、特别地片状阻挡材料的掺杂涂层。
胶带粘合剂将至少一个载体和阻挡材料连接在固体绝缘材料中。它以1-30重量％、优选地2-15重量％、特别优选地5-10重量％的量存在于固体绝缘材料中。
根据本发明的有利的实施方式，固化催化剂(亦称为“带固化催化剂”或“带促进剂”)以小于10重量％、例如0.001重量％至7.5重量％、优选地在0.01重量％至5重量％的范围内、特别优选地0.1重量％至3.5重量％的浓度存在于固体绝缘材料中，使得可实现几小时的凝胶化时间。
根据本发明的有利的实施方式，固化催化剂在20℃至100℃、优选地50℃至80℃且特别优选地55℃至75℃的范围内的温度下引发浸渍树脂的聚合。
为了在固体绝缘材料中实现所要求的储存稳定性，例如在室温下且别地在连续保持几小时的真空和浸渍温度，固化催化剂是对胶带粘合剂材料比较惰性的。在例如在20℃和100℃的范围内、特别地在50℃至80℃的范围内、最优选地在55℃至75℃之间的保持真空和/或浸渍温度的条件下尤其如此。适合作为胶带粘合剂的是例如二醇、三醇和/或多元醇。
本发明涉及固体绝缘材料、特别地带形式(带状)的固体绝缘材料、其在真空浸渍工艺中的用途和由其制造的绝缘体系以及具有该绝缘体系的电机，特别地用于中压和高压范围，即用于中压和高压机器、尤其是在中压和高压范围内的旋转电机以及用于电气开关装置的半成品。所述固体绝缘材料和由其制造的绝缘体系的特征在于，它可以无酸酐的方式制备，其中固化催化剂例如是1H-咪唑和/或1H-咪唑衍生物与含环氧乙烷基团的化合物的加合物。

Claims (22)

1.固体绝缘材料，其能在真空浸渍工艺中与不含酸酐的浸渍剂一起用于制造绝缘体系，其中所述固体绝缘材料包括载体、阻挡材料、固化催化剂和胶带粘合剂，所述固化催化剂和胶带粘合剂相对于彼此呈惰性，但在真空浸渍条件下与不含酸酐的浸渍剂以1小时至15小时的凝胶化时间在浸渍温度下反应，其中固化催化剂通过至少一种1H-咪唑和/或1H-咪唑衍生物与包含环氧乙烷基团的化合物反应而获得。
2.根据权利要求1的绝缘材料，其中所述包含环氧乙烷基团的化合物每分子具有n＝1-4个环氧乙烷官能度。
3.根据权利要求1或2的绝缘材料，其中所述包含环氧乙烷基团的化合物是缩水甘油基化合物。
4.根据前述权利要求之一的绝缘材料，其中所述包含环氧乙烷基团的化合物在室温下以液体形式存在。
5.根据前述权利要求之一的绝缘材料，其中所述固化催化剂为如下的化合物，其为一种和/或多种1H-酸二氮杂环和/或1H-酸三氮杂环与所述包含环氧乙烷基团的化合物的加合物。
6.根据前述权利要求之一的绝缘材料，其中所述包含环氧乙烷基团的化合物包括选自以下化合物的组的化合物：
单缩水甘油醚和/或酯化合物(n＝1)，
二缩水甘油醚和/或酯化合物(n＝2)，
三缩水甘油醚和/或酯化合物(n＝3)和/或
四缩水甘油醚和/或酯化合物(n＝4)，以及所述化合物的任何所需的混合物。
7.根据前述权利要求之一的绝缘材料，其中所述固化催化剂具有例如在1至15mmol/g的范围内的氮密度D。
8.根据前述权利要求之一的绝缘材料，其中所述固化催化剂为以下与所述包含环氧乙烷基团的化合物的加合物：
1H-2-甲基咪唑(CAS号693-98-1)，
1H-2-乙基咪唑(CAS号1072-62-4)，
1H-4-乙基-2-苯基咪唑，
1H-3,5-二甲基吡唑，
1H-咪唑(CAS号288-32-4)，
1H-4(5)-甲基咪唑(CAS号822-36-6)，
1H-2-乙基-4-甲基咪唑(CAS号931-36-2)，
1H-4-甲基-2-苯基咪唑(CAS号827-43-0)，
1H-4-苯基咪唑(CAS号670-95-1)，
1H-5-甲基-2-苯基咪唑-4-甲醇(CAS号13682-32-1)，
1H-吡唑(CAS号288-13-1)，
1H-3-苯基吡唑(CAS号2458-26-6)，
1H-5-甲基吡唑，
1H-3,4-二甲基吡唑(CAS号2820-37-3)，
1H-3,5-二甲基吡唑(CAS号67-51-6)，
1H-3-叔丁基吡唑(CAS号15802-80-9)和/或
1H-4-乙基吡唑(CAS号17072-38-7)
以及任何所需的上述化合物的混合物。
9.根据前述权利要求之一的绝缘材料，其中所述固化催化剂每分子另外具有n＝1-4个共价键合的羟基基团。
10.根据前述权利要求之一的绝缘材料，其中胶带粘合剂包括以下称为链段“A(OH)n”的双酚、二元醇、三元醇和/或更高级的醇与以下称为链段“Cy”的氧化环己烯和/或氧化环己烯衍生物的加合产物，其中A(OH)n选自以下化合物：
-单乙二醇(C2H4)(OH)2；丁二醇(C4H8)(OH)2；丁烯二醇(C4H6)(OH)2；丁炔二醇(C4H4)(OH)2；聚乙二醇H(OC2H4)x(OH)2，其中x＝1至5000；丙烷二醇(C3H6)(OH)2；聚丙二醇H(OC3H6)x(OH)2，其中x＝1至5000；二甘醇(C2H8O)(OH)2；丙二醇(C3H6)(OH)2；新戊二醇(C5H10)(OH)2；环戊二醇(C5H8)(OH)2；环戊烯二醇(C5H6)(OH)2；甘油(C3H5)(OH)3；戊二醇(C5H10(OH)2；季戊四醇(C5H8)(OH)4；己烷二醇(C6H12)(OH)2；己二醇(C6H12)(OH)2；庚二醇(C7H14)(OH)2；辛二醇(C8H16)(OH)2；聚己内酯二醇；聚己内酯三醇；氢醌(C6H4)(OH)2；间苯二酚(C6H4)(OH)2；(焦)儿茶酚(C6H4)(OH)2；白藜芦醇(C10H12)(OH)2；三甘醇(C6H12)(OH)2，
-完全芳族的、部分氢化的和/或完全氢化的双酚A(C15H14)(OH)2，(C15H28)(OH)2，双酚F(C13H10)(OH)2，双酚S(C12H8O2S)(OH)2，
-三环癸烷二甲醇(C12H18)(OH)2，甘油碳酸酯(C4H5)(OH)1。
11.根据前述权利要求之一的绝缘材料，其包括选自以下化合物的组的化合物作为胶带粘合剂:
三环甲烷二甲醇(CAS号26896-48-0或26160-83-8)，
三羟甲基丙烷(CAS号77-99-6)，
枝状羟基官能聚合物(CAS号326794-48-3或462113-22-0)，
聚己内酯三醇(CAS号37625-56-2)，
聚己内酯四醇(CAS号35484-93-6)。
12.根据前述权利要求之一的绝缘材料，其以小于10重量％的量包含所述固化催化剂。
13.根据前述权利要求之一的绝缘材料，其以在1至30重量％的范围内的量包含所述胶带粘合剂。
14.根据前述权利要求之一的绝缘材料，其包括以织造织物、非织造织物和/或膜形式的载体。
15.根据权利要求10所述的绝缘材料，其包括穿孔膜。
16.根据前述权利要求之一所述的绝缘材料，其包括颗粒状的阻挡材料。
17.根据前述权利要求之一所述的绝缘材料，其中所述颗粒状的阻挡材料至少部分地包括片状的阻挡材料颗粒。
18.根据权利要求12或13所述的绝缘材料，其中阻挡材料的颗粒是经涂覆的。
19.根据权利要求12至14之一所述的固体绝缘材料，其中涂料包括金属氧化物。
20.根据权利要求12至15之一所述的固体绝缘材料，其中涂料是经掺杂的。
21.用根据权利要求1至20之一所述的固体绝缘材料通过真空浸渍制造的绝缘体系在中压和高压机器、特别地中压和高压范围内的旋转电机中，以及在电气开关设备、中压和高压应用、套管、变压器套管、发电机套管和/或套管中，以及在相应的半成品中的用途。
22.电机、优选地旋转电机、特别优选地在中压和高压范围内的旋转电机以及电气开关设备、中压和高压应用、套管、变压器套管、发电机套管和/或套管以及相应的半成品，其包括由根据权利要求1至20之一所述的固体绝缘材料制造的绝缘体系。
CN201780016081.6A 2016-03-09 2017-02-08 固体绝缘材料、其用途和由其制造的绝缘体系 Expired - Fee Related CN108780675B (zh)

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