CN1026277C - 制造用于导电体的绝缘层的绝缘带 - Google Patents

制造用于导电体的绝缘层的绝缘带 Download PDF

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CN1026277C
CN1026277C CN89109783A CN89100727A CN1026277C CN 1026277 C CN1026277 C CN 1026277C CN 89109783 A CN89109783 A CN 89109783A CN 89100727 A CN89100727 A CN 89100727A CN 1026277 C CN1026277 C CN 1026277C
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沃尔夫冈·罗格勒
弗兰茨-约瑟夫·扑尔迈尔
沃尔特·伊莱恩
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Abstract

制造用于导电体的热硬化环氧树脂—酸酐混合物浸渍绝缘层的绝缘带。
用于制造绝缘层(5)的该绝缘带(1)由耐压无机材料制成，由粘结剂粘合在揉韧的村底(2)上，该绝缘带还含有加速硬化反应的促进剂，粘结剂-促进剂混合物在浸渍树脂硬化温度时形成自硬化系统。

Description

本发明涉及制造用于导电体的热硬化环氧树脂-酸酐混合物浸渍绝缘层，尤指电机上的绕组杆和线圈用的绝缘带，这种绝缘带是由铺设在揉韧衬底上的耐压扁平无机材料构成，如小块云母片或颗粒云母层，并且用粘结剂与衬底粘合在一起，需要时可与复盖层密封，该绝缘带还包括加速浸渍树脂混合物硬化反应的促进剂，粘结剂-促进剂混合物构成在浸渍树脂硬化温度时的自硬化系统。
正如DE-PS2142571时公开的，这种绝缘带能够很容易进行浸渍，因为所采用的浸渍树脂混合物不易起反应，在保证绝缘层良好浸渍的高温下，实际上也并未改变其粘度。这是合乎需要的，因为用作浸渍树脂的环氧树脂-酸酐混合物只有少量浸入绝缘层，而剩余的混合物仍可重新用于浸渍。因此，绝缘带包括加速浸渍树脂硬化反应的促进剂，使浸入绝缘层的浸渍树脂在很短的时间内即能硬化。
为了使绝缘带在浸渍前能够存放很长时间，已知绝缘带选用的粘结剂-促进剂混合物应是在室温条件下实际上不会硬化的这类混合物。此外，粘接剂-促进剂混合物成自硬化系统，也只有在显著超过室温的浸渍树脂硬化温度条件下才有可能。这样才能避免浸入耐压无机材料层之间的粘结剂完全不被浸渍树脂吸收，而且在绝缘体中保持不硬化。
已知绝缘带所用的粘结剂是当量在180以下的环脂族环氧树脂，其环氧基是由氧原子接在环的双键上形成的。如通常所知，这说明胺类硬化剂和促进剂没有反应，或反应很慢。但是加入环氧树脂-酸酐浸渍树 脂时，这种促进剂的催化活性充分提高。已知绝缘带所用的促进剂包括摩尔比为1∶1的二氧化乙烯基环己烯和仲胺的加合物（其仲氮原子是加氢环系中的一个环）和摩尔比为1∶1的二氧化乙烯环己烯和1位上没有被取代的咪唑的加合物。
但最近的研究业已证明，二氧化乙烯基环己烯（4-乙烯基-1.2环己烯二环氧化物）被认为是一种有害健康的物质，因为它在动物试验中证明具有致癌作用。
根据制造者的归类，环脂族环氧树脂（3（3′，4′-环氧环己基）-7，8-环氧-2，4-氧杂螺双环[5，5]十一烷（环氧化物当量约162）也属于这一类。
因此，本发明的任务在于提供一种用于上述绝缘带的粘结剂-促进剂体系，而且根据迄今所知的全部研究证明是无害于健康的。
为了解决上述任务，用于上述本发明绝缘带的粘结剂是一种无害于健康的环氧化的通过增加分子进行改性的环脂族环氧树脂，其环氧化物的当量大于200，所用的促进剂是由1位上取代的哌嗪和（甲基）丙烯酸酯化合物构成的加合物。
根据本发明制造的绝缘带，在室温条件下可储放三个月以上而不发生性质变化。在一个化合物与可进行加成反应的复合物进行加成反应得到的哌嗪加合物用作促进剂时，使环氧树脂-酸酐混合物在60℃时就能促进并大大加速其胶凝化，从而能使浸入绝缘层的浸渍树脂在很短的时间内硬化。按本发明加到粘结剂中的促进剂体系与粘结剂相比，在相同时间反应速度都较低，但与浸入的浸渍树脂相比，反应速度还是较高，除此之外，还有一个重要的优点，就是在高至80℃的温度范围内，蒸汽压特别低，因此在真空压浸渍（VPI工气）条件下，也不会因加速和激化粘结剂-促进剂混合物中作用成分的蒸发而产生热硬化环氧树脂-酸酐混合物影响的危险。
按本发明方法制造的粘结剂-促进剂体系即使在绝缘层浸渍前对缠绕着绝缘带的绝缘层进行干燥和预热时，也能确保在浸渍树脂中充分溶解，与在浸渍过程中浸入绝缘层的浸渍树脂相比，反应速度也不会下降。
基于反应速度考虑，值得介绍的促进剂是由1Mol丙三丙烯酸三羟甲酯（Trimethylopropantriacrylat）和3Mol在1位上取代的哌嗪（如1-甲基哌嗪或1-乙基哌嗪）反应得到的产物。
根据本发明制造的绝缘带，其所用粘结剂可以（3，4-环氧）环己烷羧酸3，4-环氧环己基甲基酯或己二酸双（3，4-环氧环己基甲基）酯为基础，通过将分子增加至使环氧化物当量大于200获得改性的环氧化环脂族环氧树脂。这两种树脂的改性是绝对必要的，因为在粘度约为350毫泊/25℃（当量140）或粘度约为700毫泊/25℃（当量约为208）时，如不增加分子而要制造可以进行涂覆加工的绝缘带，则这样的树脂的粘着力实在太小了。为了通过增加分子获得高粘度的化合物，主要有如下三种已知方法可以提供：
a）采用相应的促进剂进行离子聚合;
b）过量酐的加成，即在形成酯基的情况下增加分子;
c）在形成芳香基-醚结构的条件下，特殊芳香二醇的加成（先进方法）。
具有特殊优点的本发明绝缘带的粘结剂是按方法c）与双酚A反应制造的产物，其中尤其是环氧化物当量约为250的（3，4-环氧）-环己烷羧酸3，4-环氧环己基甲基酯和当量接近500的己二酸双（3，4-环氧环己基甲基）酯的加成产物，它们的粘度较高，粘合力极好。
用于该反应的催化剂是由先进方法得知的一组化合物，如季铵盐、季鏻盐、有机膦等。这类催化剂体系的实例在专利文件E-PS-009334和US-PS-4389520中已有介绍。其中证明有效的化合物如：苄基三乙基氯化铵和苄基二甲基十四烷基氯化铵。
在制造绝缘带时，为使浸渍树脂在浸渍时能很好地浸入绝缘带中的空腔，选择粘结剂的量不可过大。因此，以绝缘带的总重量为基准，用作粘合绝缘带粘结剂的化合物的重量约为3-20%。采用这样重量的粘结剂时，以绝缘带的总量为基准，确定促进剂的量约为0.05-3%。制造时加入到绝缘带中的促进剂的量决定于无机材料的多少（例如绝缘带中每个衬底中含有多少云母）和绝缘带中用于粘合的粘结剂的量有多大。
进一步改进按本发明方法具有高刚性的绝缘带，可以通过使粘结剂-促进剂混合物含有起硬化剂作用的混合物，它们在热硬化环氧树脂-酸酐混合物的硬化温度下能够发挥作用，从而进一步提高自硬化粘结剂的耐热形变的能力。但是这些混合物不能影响绝缘带的储存能力。这些含有混合物的粘结剂-促进剂混合物在绝缘带浸渍前进行干燥和预热的条件下仍能充分溶解于浸渍树脂中。
特别适合的起硬化剂作用的混合物应在高至80℃时仍不溶于粘结剂中并且要有足够高的熔点，例如2-苯基-4，5-二羟基甲基咪唑。这种混合物在硬化温度时仍显示其活性。当在60℃时，粘结剂中哌嗪-丙三丙烯酸三羟甲酯加合物能加速浸入绝缘层的浸渍树脂的胶凝化。
此外，复杂化合物或加合物也适宜于用作混合物，它们在硬化温度时能分解成起硬化作用的组分。这类化合物，例如在DE-OS-2811764中已有介绍，或者是1，2，4-苯三酸与咪唑反应生成的盐，例如1-氰基乙基-2-甲基咪唑-（1，2，4-苯三酸）。
包在囊内的或吸附在具有很大活性表面的物质上的硬化剂体系也适宜于用作混合物，它们在硬化温度时或通过与其他化合物的交换能够释放并且产生作用，例如可以采用吸附在分子筛中的叔胺。混合到粘结剂中的这类硬化剂的用量决定于它们特异的功效，但以粘结剂为基准，应在0.05-10（重量）%范围之内。
下面将根据表1至4详细说明本发明的内容：
表1给出三种不同混合物由双酚A和相应的环氧化环氧树脂反应得到的产物制造的绝缘带的工艺数据。其中第1列中的A表示3，4-环氧环己基甲基-3，4-环氧环己烷羧酸甲酯;B表示双（3，4-环氧环己基甲基）己二酸。
表1
双酚A的含量    70℃时反应    反应产物
环氧    （以环氧树脂的    产物的粘度    中的环氧    反应产物
树脂    重量100为基准）    （毫泊）    化物数    种类
21 约5000 0.43 A1
A 23 约10000 0.40 A2
25 约18000 0.38 A3
19 约4000 0.26 B1
B 23 约15000 0.21 B2
25 约20000 0.21 B3
按照在50°-70℃下具有较高粘合力和在浸渍树脂-硬化剂混合物中具有较高溶解度的情况，优先对反应产物A和B作进一步研究。
表2给出三种不同粘结剂-促进剂混合物放置在敞开容器中的储放能力。
促进剂1：由1Mol丙三丙烯酸三羟甲酯（TMPT）和3Mol    1-甲基哌嗪得到的加成产物。
促进剂2：由1Mol    TMPT和3Mol    1-乙基哌嗪得到的加成产物。
为了进行研究，促进剂在加温条件下（70℃）或采用MeCl2作为溶剂，溶于粘结剂树脂A和B中。
表2中，第Ⅰ列是粘结剂的种类，第Ⅱ列是促进剂的种类，第Ⅲ列是促进剂的重量（以粘结剂的重量100为基准）。
表2
Ⅰ    Ⅱ    Ⅲ    在70℃储存后，70℃时混合物的粘度（毫泊）
AW    1周    2周    3周    4周
A    1    10    13000    90000    31000    70℃测不到，
但未凝胶
A    2    15    10000    14500    19000    29000    33000    10周后
约300000
B    2    15    12000    15000    16000    18000    19000    10周后
约300000
与由1Mol    TMPT和3Mol    1-甲基哌嗪（促进剂1）得到的加成产物相比，由1-乙基哌嗪得到的加成产物在70℃时，由于粘结剂树脂的离子聚合催化活性明显较低。
表3给出所研究的粘结剂-促进剂混合物对环氧树脂-酸酐混合物具有明显的促进作用。试验采用双酚A（环氧化物当量174±2）的缩水甘油醚和甲基六氢邻苯二甲酸酐的环氧树酯-酸酐混合物。
表3中，第Ⅰ列是粘结剂-促进剂混合物，第Ⅱ列是粘结剂-促进剂混合物的重量（以环氧树脂-酸酐的重量100为基准）。
表3
Ⅰ    Ⅱ    环氧树脂-酸酐-促进剂混合物的胶凝时间（分钟）
70℃    90℃
A31 22 100 26
A32 23 125 28
B32 23 130 30
1-甲基-哌嗪加合物与1-乙基-哌嗪加合物相比，二者的反应速度都较快，其区别在于促进剂对浸渍树脂体系的作用小于对相应的粘结剂系统的催化作用（见表2）。因此，如果考虑粘结剂-促进剂混合物的储 存能力和促进剂对浸渍树脂系统的作用这两个重要性质，那么首先1-乙基-哌嗪加合物具有所需要的性质。
表4给出粘结剂-促进剂混合物的储放稳定性的数据，它们是由10份（重量）的粘结剂2（由1Mol    TMPT和3Mol    1-乙基哌嗪得到的加成产物））以粘结剂A的重量100为基准，见表1）构成，其作为混合物的是2个特异硬化剂，即：1＝2苯基-4，5-二羟基甲基咪唑，或2＝1氰基乙基-2-苯基咪唑-（1，2，4-苯三酸）。
表4中，第Ⅰ列是所用的硬化剂，第Ⅱ列是硬化剂的重量（以粘结剂的重量100为基准）。
表4
混合物的储放稳定性（天）    130℃时的胶凝
Ⅰ    Ⅱ    室温    70℃    时间（小时）
1    3    150    10    约16
2    3    150    8    约12
从表4中可见，温度至70℃时，加入的混合物对粘结剂-促进剂混合物提高反应速度很小。在这个温度范围内，与表2相比，总的反应速度略高，但是在室温条件下，混合物的稳定性极好。
通过加入混合物，将硬化的粘结剂的玻璃点（Glaspunkt）提高大约30℃，那么缠绕着绝缘带的绝缘层的刚性可进一步提高，在较高温度时，其机械强度也可进一步提高。
图1和图2中按本发明制造的绝缘带是以图示实施例用以进一步说明本发明。图3表示缠着绝缘带的经过浸渍和硬化的绝缘层的刚性与温度的函数关系。
绝缘带1由一个柔韧的衬底2即用作载体的玻璃织物构成，但也可采用人造纤维织物和人造纤维布，或采用特别耐高温的塑料薄膜。
在衬底2上铺设一层小块云母片3。为了把衬底2与云母层3粘结 在一起，采用由粘结剂A（见表1）和（由1Mol    TMPT与3Mol    1-乙基哌嗪制成的）加合物作为促进剂制成的快速粘结剂。也可用快速粘结剂将云母纸或玻璃薄片粘结在衬底2上，而不用云母层3。云母层3用与衬底相同的材料制成的复盖层封闭。但复盖层也可用其它揉韧材料制成。这样制造的绝缘带1在25℃条件下能储存三个月以上。
为了制造绝缘层5，在电机的导体上，如在绕组杆或如图中所示带绕组线段绝缘的线圈6上，用绝缘带1重叠缠绕。可缠绕许多层直至绝缘层5达到所需的强度。然后按VPI工艺，将带有绝缘层5的线圈6用环氧树脂-酸酐硬化剂混合物浸渍，硬化。
为了研究图3所示绝缘层5的力学刚性与温度的关系，将大约2mm厚即用12层100μ厚的云母纸复合的试验样品缠绕，并用单位面积重量约为28g/cm2的玻璃织物缠绕和在70℃下用双酚A-环氧树脂-甲基六氢邻苯二甲酸酐-浸渍树脂混合物浸渍。在140℃下硬化24小时。图3的横座标为温度，用℃表示，纵座标为力学刚性，即杨氏模数，用GPa表示。
曲线7表示用由DE-PS    2142571公开的云母缠绕的绝缘层的刚性。
曲线8和9表示用由含本发明的粘结剂-促进剂混合物的云母带缠绕的绝缘层的刚性。曲线8的绝缘层含有粘结剂A（见表1），曲线9的绝缘层含有粘结剂B。这两个情况都采用1Mol    TMPT和3Mol    1-乙基哌嗪的加合物作为促进剂。
根据测定值，曲线7和8所代表的绝缘层，抗热变形较高，而曲线9由于粘结剂树脂中残余己二酸的揉曲作用，未能完全达到这样高的值。

Claims (12)

1、制造用于导电体，尤指用于电机上的绕组杆和线圈的热硬化环氧树脂-酸酐混合物浸渍绝缘层的绝缘带，所述绝缘带是由铺设在揉韧衬底上的耐压扁平无机材料制成，如小块云母片或颗粒云母层，并用粘结剂与衬底粘合在一起，需要时可与复盖层密封，该绝缘带还含有加速浸渍树脂混合物硬化反应的促进剂，粘合剂-促进剂混合物构成在浸渍树脂硬化温度时的自硬化系统，其特征在于所用粘结剂是一种对生理无害的、环氧化的、经过增加分子而得到改性的环氧化物当量大于200的环脂族环氧树脂，所用促进剂是一种1位被取代的哌嗪和(甲基)丙烯酸酯化合物的加合物。
2、按权利要求1的绝缘带，其特征在于所用粘结剂是一种通过增加分子至环氧化物当量大于200而改性的3，4-环氧环己基甲基（3，4-环氧）环己烷羧酸。
3、按权利要求1的绝缘带，其特征在于所用粘结剂是一种通过增加分子至环氧化物当量大于300而改性的双（3，4-环氧环己基甲基）己二酸。
4、按权利要求1、2或3的绝缘带，其特征在于按照先进方法，粘结剂通过与双酚A反应增加分子。
5、按权利要求1的绝缘带，其特征在于所用促进剂是由1摩尔丙三丙烯酸三羟甲酯和3摩尔1-乙基-哌嗪反应得到的产物。
6、按权利要求1的绝缘带，其特征在于所用促进剂是由1摩尔丙三丙烯酸三羟甲酯和3摩尔1-甲基-哌嗪反应得到的产物。
7、按权利要求1的绝缘带，其特征在于粘结剂-促进剂混合物含有起硬化剂作用的混合物，其仅在硬化温度时才对热硬化环氧树脂-酸酐混合物起作用。
8、按权利要求7的绝缘带，其特征在于将2-苯基-4，5-二羟甲基咪唑作为混合物加入到粘结剂-促进剂混合物中。
9、按权利要求7的绝缘带，其特征在于将1-氰基乙基-2-甲基咪唑-（1，2，4-苯三酸）加入到粘结剂-促进剂混合物中。
10、按权利要求1、2或3的绝缘带，其特征在于粘结剂的重量为绝缘带总重量的3-20%。
11、按权利要求1、5或6的绝缘带，其特征在于促进剂的重量约为绝缘带总重量的0.05-3%。
12、按权利要求7至9之一的绝缘带，其特征在于作为混合物加到粘结剂-促进剂混合物中的硬化剂的重量占粘结剂总重量的0.05-10%。
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EP0424376B1 (de) 1993-04-07
JPH03506091A (ja) 1991-12-26
NO910148D0 (no) 1991-01-14
ZA895297B (en) 1990-03-28
WO1990000802A1 (de) 1990-01-25
NO910148L (no) 1991-03-14
AR247642A1 (es) 1995-01-31
IN171445B (zh) 1992-10-17
DE3880156D1 (de) 1993-05-13
US5158826A (en) 1992-10-27
JP2635146B2 (ja) 1997-07-30
EP0424376A1 (de) 1991-05-02
DE3824254A1 (de) 1990-01-18
BR8807913A (pt) 1991-05-14
ATE88034T1 (de) 1993-04-15
CN1039322A (zh) 1990-01-31

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