CN110072923A - 用于绝缘带的组合物 - Google Patents
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Abstract
本发明涉及一种用于制备绝缘带的组合物,其中该组合物用于将非传导材料固定到增强层上。为了提供绝缘带,其特别是在VPI方法中用于制备中压或高压装置的绝缘物,避免使用常规固化剂,特别是羧酸酐,建议了一种组合物,该组合物包含:a)通过取代的或者未取代的酚与醛缩合所制备的酚醛树脂,其中该酚醛树脂的分子量是250‑1000g/mol,和b)选自硼(III)卤化物和/或其胺络合物、咪唑、乙酰基丙酮酸酯,氯化锡(IV)和/或叔胺和/或四甲基胍的催化剂,和c)任选的其他添加剂。
Description
本发明涉及一种用于制备绝缘带的组合物,其中该组合物用于将非传导材料固定到增强层上,和涉及其用途。
高压装置例如电动机或者发电机中的绝缘系统目的在于提供导电部件例如电线,线圈或者棒材相比于彼此和相对于定片芯组或者环境的耐久的电绝缘。通常在这些绝缘系统中存在的问题是由于雪崩式电荷迁移而发生局部放电,其最终可能造成绝缘体的电击穿。为了抵抗这个问题,用云母带缠绕待绝缘的零件,并且其应在火灾事件中保持导体的功能。将经常由云母浆(包含白云母和金云母)借助粘结剂所制备的云母纸与牢固的载体带,例如由例如,玻璃,岩棉,聚酯或者聚酰亚胺制得的织造织物,非织造织物或者箔借助粘合剂粘合来制备云母带。云母纸可以在一侧或者两侧上设有载体带,其中该侧面也可以由不同的载体材料组成。以如下方式进行粘合,使用粘结剂来渗透云母纸和载体材料,和因此形成预浸料。
使用树脂组合物作为粘合剂,其在室温具有高强度来确保云母和载体的结合,并且其在高温(60℃-150℃)变成液体状态。这确保了它们可以在高温以液体粘合剂形式或者以与挥发性溶剂的混合物施加。在冷却或者除去该溶剂之后,所述粘合剂以牢固但仍挠性的形式存在,因此允许用云母带在室温可靠缠绕导电零件,其中粘合剂的粘合性能防止了该云母纸从载体材料上脱层。由现有技术(WO1998/014959A1)已知例如硅树脂,聚烯烃,聚乙烯基酯,聚乙烯醇作为粘合剂的树脂成分。但是,环氧树脂特别适于这个目的,这归因于它们的电导率参数。US5618891,US5158826,US4656090,US3647611以及WO2015/062660A1描述了用于云母带的具体环氧树脂组合物。除了环氧树脂组分之外,该粘合剂通常此外包含加速剂组分,其适于引发随后施用的基于环氧树脂的浸渍树脂(例如酸酐固化)的硬化过程,其中仅仅特定选择的加速剂适于这个目的,因为必须避免在云母带上过早硬化,例如在云母带存储期间或者在浸渍工艺过程中。
用云母带缠绕的导体通常优选用合成树脂在真空-压力-浸渍方法(VPI方法)中进行浸渍。
在该真空-压力-浸渍方法中在第一步骤中,借助真空来蒸发来自位于浸渍容器中待浸渍的用云母带缠绕的导体的残湿,和在随后的第二步骤中,将所述的缠绕物首先在负压下并且随后在压力下用来自于储备容器的浸渍树脂淹没。因此可以实现绝缘系统的完全渗透。可以借助电容测量来监控该绝缘系统的树脂吸收。当电容变化已经达到最小值时终止所述方法。可以借助在所述容器中占优的压力驱使浸渍树脂返回储备容器。在滴干后,将所述产物转移到干燥烘箱,在其中进行硬化。作为浸渍树脂主要使用基于环氧树脂的树脂,因为其中可以放弃额外的溶剂。这些树脂此外具有良好的耐真空性,低的体积收缩率和与云母带高的粘合强度。为了使得环氧树脂具有适于所述方法的粘度,将它保持在60℃-70℃温度的浸渍容器中。然而其要求固化剂(其处于在浸渍容器中与环氧树脂组分的混合物中)其在所述温度是非反应性的,而是在硬化方法的明显较高温度(>120℃)才是反应性的。该固化剂此外必须确保浸渍周期短,并且在浸渍程序之后滴落损失小。固化剂因此,羧酸酐例如六氢邻苯二甲酸酐(HHPA)或甲基六氢邻苯二甲酸酐(MHHPA)适于作为固化剂用于基于环氧树脂的浸渍树脂,但是其被怀疑对健康有害,因此应当从所述制备方法中排除。
因此,本发明的一个目的是提供一种绝缘带,优选云母带,其特别是当用于VPI方法中制备中压和高压装置的绝缘物时,避免了使用常规的固化剂,特别是羧酸酐。
所述目的根据本发明通过一种用于制备绝缘带的组合物来实现,其中该组合物用于将非传导材料固定到增强层上,特征在于,该组合物包含:
a)通过取代的或者未取代的酚与醛缩合所制备的酚醛树脂,其中该酚醛树脂的分子量是250-1000g/mol,和
b)选自硼(III)卤化物和/或其胺络合物、咪唑、乙酰基丙酮酸酯,氯化锡(IV)和/或叔胺和/或四甲基胍的催化剂,和
c)任选的其他添加剂。
本发明的组合物作为非传导材料(优选云母)之间的粘合剂,以常规方式,借助喷涂、涂抹或刮涂施加到增强层上,即载体带上,其优选由如下形成:由玻璃和/或岩棉和/或聚酰亚胺和/或聚酯和/或石英制成的织造织物、编织织物、非织造织物或者箔。这产生了由在一侧或多侧上用增强层涂覆的云母纸制成的整面用本发明组合物浸渍的复合材料。该绝缘带优选包含5-20重量%的本发明的粘合剂,基于总质量(载体带,非传导材料,粘合剂)。
由于仔细选择本发明组合物的组分和所形成的反应性,所述的复合材料在室温是存储稳定的,并且可以任选地切割成期望的带宽度和作为卷材存储。现在可以提供这样的云母带,其与上述的基于环氧树脂和引发了随后的酸酐固化的催化剂组分的云母带相比具有较好的存储稳定性。
通过具有本发明组合物的云母带可以特别是提供用于中压和高压装置的绝缘物,其具有环氧树脂作为浸渍树脂,并且有利地以VPI方法制备。在浸渍程序过程中,借助真空,将加热(约40-80℃)的基于环氧树脂的浸渍树脂浸渍用云母带缠绕的导体,其中该云母带具有本发明的组合物。本发明组合物的酚醛树脂经由云母带引入浸渍树脂的环氧树脂中,并且充当了后者的助固化剂。存在于该云母带中的催化剂用于引发浸渍树脂的均聚和加速全部的浸渍层的固化程序;由此可以优化硬化时间。
通过该云母带的本发明的组合物,可以将绝缘层的损耗因子tan(δ)保持在相应的水平,其表示转化成热所产生的电能的损耗,使得能够实现足够的绝缘性能。通过将本发明的组合物用于云母带,固化剂在环氧浸渍树脂中可以放弃使用迄今为止常规的酸酐固化剂;这从健康和环境方面是令人期望的。
用于本发明的绝缘带组合物的酚醛树脂是现有技术已知的。它们通过取代的或者未取代的酚与醛缩合来制备,其中所获得的酚醛树脂的分子量是250-1000g/mol(根据DIN55672-1测量)。优选的是单核取代的或者未取代的酚(例如苯酚,甲酚和/或对叔丁基酚)与醛(优选甲醛)在酸性中反应。这些化合物是容易获得的。最常用于酸性缩合的催化剂是草酸、盐酸、对甲苯磺酸、磷酸和硫酸。这里该反应混合物典型的摩尔比是0.75-0.85mol甲醛比1mol酚(F/P=0.75-0.85)。当分子量已经达到250-1000g/mol,优选250-500g/mol时,终止所述缩合,因为因此可以优化调节该组合物的粘度,粘度对于施用到载体带上发挥重要作用。
本发明所用的酚醛树脂是市售可得的,例如名称PH8505(HexionGmbH的产品)。
本发明的组合物此外包含催化剂,优选1-30重量%,更优选5-30重量%,基于酚醛树脂的质量,其选自硼(III)卤化物和/或其胺络合物,咪唑,乙酰基丙酮酸酯,氯化锡(IV)和/或叔胺和/或四甲基胍。优选三氟化硼络合物和三氯化硼络合物,或胺硼酸盐,但是特别优选选自咪唑,特别是2-苯基咪唑的化合物。来源于所述方法重要的是云母带中存在的催化剂具有适当的蒸气压,其一方面在云母带批量生产后不排气,和另一方面允许在VPI方法过程中迁移到浸渍树脂的浸渍层中来整体加速浸渍层的固化。这是通过有目的地选择催化剂来保证的。
作为另外的组分,本发明的组合物可以任选地包含其他添加剂例如加工助剂(例如溶剂,例如甲乙酮),增附剂(例如硅烷),或者润湿剂。这些添加剂对于绝缘带的制备和性能具有积极作用。
所述组合物因此有利地包含例如50-90重量%的酚醛树脂,1-30重量%的催化剂和0-49重量%的其他添加剂,基于该组合物所有组分的总质量。
通过包含下面步骤的方法来制备待绝缘的导体的绝缘物:
(I)提供绝缘带,其包含借助组合物彼此粘合的非传导材料和增强层,其中该组合物包含
a)通过取代的或者未取代的酚与醛的缩合制备的酚醛树脂,其中该酚醛树脂的分子量是250-1000g/mol,和
b)选自硼(III)卤化物和/或其胺络合物、咪唑、乙酰基丙酮酸酯、氯化锡(IV)和/或叔胺和/或四甲基胍的催化剂,和
c)任选的其他添加剂,
(II)用绝缘带缠绕导电体,和
(III)使用基于环氧树脂的树脂来浸渍缠绕导电体的绝缘带。
该基于环氧树脂的浸渍树脂是现有技术已知的。该树脂可以选自基于双酚A和/或F的聚环氧化物和由其制备的高级树脂,基于环氧化的卤代双酚和/或环氧化的酚醛树脂,和/或基于邻苯二甲酸、六氢邻苯二甲酸的聚环氧酯,或者基于对苯二甲酸的聚环氧酯,环氧化的间或者对氨基酚,或者由二环戊二烯和酚制得的环氧化的加聚产物。
因此,作为树脂组分的材料例如是环氧化的酚酚醛树脂(酚和例如甲醛和/或乙二醛的缩合产物),环氧化的甲酚酚醛树脂,双酚A基聚环氧化物(还有例如由双酚A和四缩水甘油基亚甲基二胺制得的产物),环氧化的卤代双酚(例如四溴双酚A基聚环氧化物)和/或双酚F基聚环氧化物,和/或基于三缩水甘油基异氰尿酸酯的环氧化的酚醛树脂和/或环氧树脂。所有这些树脂的平均分子量优选是200-4000g/mol,和环氧当量优选是100-2000g/当量。
尤其可以使用下面的树脂组分:
例如聚环氧化物,其基于双酚A(例如162或者828)和/或双酚F(例如158或者862),及其混合物,和包含反应性稀释剂的混合物(例如Modifier AQ),脂环族环氧树脂(例如760产品,可获自Hexion Inc.)。
该浸渍树脂还可以任选地包含其他组分例如润湿剂,其用于控制表面张力。还可能的是加入起固化作用的其他成分,但是其中优选应在浸渍树脂中放弃使用酸酐。
特别优选的是步骤(III)中在真空进行的浸渍(VPI方法),由此确保用浸渍树脂几乎完全浸渍了用云母带缠绕的导体制得的复合材料。视所用的浸渍树脂而定,该浸渍之后通常随后在80℃-180℃温度的干燥烘箱中硬化。
本发明将参考实施例来更详细地描述:
1.制备云母带
为了制备云母带,首先如下来配制粘合剂组分:
将1000g的酚醛树脂(PH 8505)加热到60℃和将150g的2-苯基咪唑与之混合。
将该混合物在60℃在1小时的时间内均化。然后在60℃制备在甲乙酮中的80%的溶液,并且冷却到室温。将所制得的粘合剂用于将厚度100μm的云母纸层以23g/m2的层重固定到玻璃非织造织物。为此目的,将20g/m2的粘合剂喷涂到所述玻璃非织造织物上并与该云母纸结合,并且将该复合材料在70℃真空干燥(10mbar)。
将所制得的云母带冷却到室温。
2.在VPI方法中制备浸渍系统
将如上所述制备的云母带切割成10x10cm的块。将10层云母带彼此层叠成大约2mm的层厚度,并且在两侧开放的金属模具中在40℃和5mbar,用由250g的EPIKOTETM树脂162,750g的EPIKOTETM树脂158和150g的Heloxy Modifier AQ组成的浸渍树脂在60分钟的时间内浸渍。借助6bar的过压来持续浸渍另外60分钟。
将多余的浸渍树脂排出,并且将所述金属模具转移到固化剂烘箱。固化分两阶段进行,首先在90℃进行3小时,然后在140℃进行15小时。
3.绝缘性能
由浸渍树脂和粘合剂制成的复合材料在固化后产生了下面的温度相关的损耗因子(tan(δ)):
它们处于与在浸渍树脂中包含酸酐固化剂的那些相当的水平,使得本发明的浸渍因此还提供了期望的绝缘性能。
Claims (12)
1.一种用于制备绝缘带的组合物,其中该组合物用于将非传导材料固定到增强层上,特征在于,该组合物包含:
a)通过取代的或者未取代的酚与醛缩合所制备的酚醛树脂,其中该酚醛树脂的分子量是250-1000g/mol,和
b)选自硼(III)卤化物和/或其胺络合物、咪唑、乙酰基丙酮酸酯,氯化锡(IV)和/或叔胺和/或四甲基胍的催化剂,和
c)任选的其他添加剂。
2.权利要求1的组合物,特征在于,该组合物包含50-90重量%的酚醛树脂,1-30重量%的催化剂和0-49重量%的其他添加剂,基于该组合物全部组分的总质量。
3.前述至少一项权利要求的组合物,特征在于,该组合物包含5-30重量%的催化剂,基于该酚醛树脂的重量。
4.权利要求1的组合物,特征在于,该酚醛树脂已经通过酚和/或甲酚与甲醛的缩合来制备。
5.前述至少一项权利要求的组合物,特征在于,该酚醛树脂的分子量是250-500g/mol。
6.前述至少一项权利要求的组合物,特征在于,将咪唑,优选2-苯基咪唑用作催化剂。
7.前述至少一项权利要求的组合物,特征在于,该非传导材料是云母。
8.前述至少一项权利要求的组合物,特征在于,该增强层为由玻璃和/或岩棉和/或聚酰亚胺和/或聚酯形成的织造织物、编织织物、非织造织物或者箔。
9.前述至少一项权利要求的组合物的用途,其用于制备云母带。
10.组合物的用途,其用于包含下面步骤的用于制备待绝缘导体的绝缘的方法,
(I)提供绝缘带,所述绝缘带包含借助组合物彼此粘合的非传导材料和增强层,其中该组合物包含
a)通过取代的或者未取代的酚与醛的缩合所制备的酚醛树脂,其中该酚醛树脂的分子量是250-1000g/mol,和
b)选自硼(III)卤化物和/或其胺络合物、咪唑、乙酰基丙酮酸酯、氯化锡(IV)和/或叔胺和/或四甲基胍的催化剂,和
c)任选的其他添加剂,
(II)用绝缘带缠绕导电体,和
(III)使用基于环氧树脂的树脂来浸渍缠绕导电体的绝缘带。
11.权利要求10的用途,特征在于,使用真空-压力-浸渍方法使待绝缘的导体绝缘。
12.前述至少一项权利要求的组合物的用途,其用于中压和高压装置,特别是发电机和电动机的绝缘。
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