CN116333657A - 叠层母排用绝缘阻燃胶膜及其制备方法 - Google Patents
叠层母排用绝缘阻燃胶膜及其制备方法 Download PDFInfo
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Abstract
本发明涉及绝缘阻燃胶膜领域,公开了叠层母排用绝缘阻燃胶膜及其制备方法;本发明制备两种中温固化剂:改性异氰酸酯A与B,并按照一定的比例与高温固化剂二氨基二苯砜混合得到复合固化剂,一方面改善了单一固化剂的缺点,降低了压合温度并提高了对金属材料的粘接力,同时改性异氰酸酯能够增韧环氧树脂改善了固化后胶膜脆的缺点。
Description
技术领域
本发明涉及纱管纸技术领域,具体为叠层母排用绝缘阻燃胶膜及其制备方法。
背景技术
叠层母排即复合母排,是一种复合结构连接排,是一种配点系统的高速公路。与传统的、复杂的、冗长的配电方式相比,叠层母排线可以支持现代化的,快速安装、便于设计和结构简洁的配电系统。它具有可重复电气性能、低电感、低阻抗、抗干扰、可靠性高、节省空间、装配简洁、快捷的特点。随着新能源汽车的不断普及,叠层母排产品作为高效可靠电气连接部件,在电子产品领域得到广泛应用。
叠层母排线用绝缘胶膜主要是由绝缘薄膜以及在其表面的粘合剂所组成,目前而言,用于粘合剂主要两种类型,分别是聚酯树脂类粘合剂和环氧类粘合剂。
聚酯类胶黏剂是一类热塑性树脂胶黏剂,虽然具有储存期长、与铜排热压后无需后固化等优点,但是热塑性饱和聚酯类胶黏剂高温剥离强度和尺寸稳定性一般较差,容易在高温高湿条件下,水解成酸,易腐蚀铜排,导致电器稳定性差也难以满足叠层母排用绝缘胶膜的要求。
环氧树脂类胶黏剂虽然具有粘结强度高、电绝缘性能好、介电性能优异、耐热性好、尺寸稳定性好等优点,但是也不可避免的具有储存期短、固化物脆且与铜排热压后需要后固化等缺点使得环氧树脂胶黏剂在叠层母排用绝缘胶膜中的应用受到限制。同时快速固化胶的固化速度与储存期之间的矛盾,一直是胶粘剂研究的难题,固化速度越快,胶粘剂的活性越大,则胶粘剂的适用期及储存期越短。
CN104178044A公开了一种环氧改性饱和聚酯树脂胶黏剂,由以下质量百分数的各组分制备而成:饱和聚酯树脂A20%~50%,饱和聚酯树脂B5%~30%,环氧树脂2%~20%,异氰酸酯1%~10%,阻燃剂20%~70%,分散剂0.05%~5%,按上述配比分散于有机溶剂中,得到叠层母排用环氧改性饱和聚酯胶黏剂。饱和聚酯体系中添加环氧树脂改性,可提高饱和聚酯胶黏剂的耐高温性能,但是也会导致叠层母排用绝缘胶黏剂变脆,且储存性能下降。
CN 106700509 A提供一种无卤热塑性树脂组合物,按照质量份数计,所述无卤热塑性树脂组合物包括共聚酰胺树脂40~80份、饱和聚酯树脂5~35份、相容剂1~10份、无卤阻燃剂10~150份及抗氧剂0.1~1份。无卤热塑性树脂组合物以饱和聚酯树脂与共聚酰胺树脂作为主体树脂得到的无卤热塑性树脂组合物,无卤环保,不含固化剂,高温流动性佳,满足低温压合要求,可用于叠层母排用胶粘剂,制备的叠层母排用绝缘胶膜具有优异的高温剥离强度、高低温冲击性能和加工性能。
发明内容
本发明的目的在于提供叠层母排用绝缘阻燃胶膜及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
叠层母排用绝缘阻燃胶膜的制备方法,包括以下步骤:
S1:将改性多异氰酸酯和二氨基二苯砜加入溶剂中,混合均匀,得到复合固化剂;
S2:将气相二氧化硅、无卤阻燃剂均匀分散在环氧树脂中,并依次加入环氧酚醛树脂、复合固化剂和溶剂,混合均匀,得到混合胶液;涂布于薄膜上,烘干,得到叠层母排用绝缘阻燃胶膜。
进一步的,所述步骤S1中,改性多异氰酸酯:二氨基二苯砜的质量比为1∶1-4∶1;其中,所述改性多异氰酸酯为改性多异氰酸酯A和改性多异氰酸酯B的混合物,改性多异氰酸酯A:改性多异氰酸酯B的质量比为1∶9-9∶1。
进一步的,所述步骤S1中,溶剂为丁酮、乙酸乙酯、甲苯或异丙醇中的至少一种。
进一步的,所述改性多异氰酸酯A为分子量在4000-9000的端羟基聚丙烯酸甲酯-丙烯酸丁酯与芳香族异氰酸酯按照异氰酸指数R在1-2范围内于45℃下反应至粘度达到20000cps~50000cps制得,在中等温度下可以作为环氧树脂的固化剂。
进一步的,所述改性多异氰酸酯B为羟值3-6的聚酯与芳香族异氰酸酯按照异氰酸指数R在1-2范围于45℃下反应至粘度达到45000-70000cps制得,在中等温度下可以作为环氧树脂的固化剂。
进一步的,所述叠层母排用绝缘阻燃胶膜中,按质量份数计,包括以下组分:
复合固化剂5-15份,气相二氧化硅0.1-3份,无卤素阻燃剂0-30份,环氧树脂10-50份,环氧酚醛树脂5-25份,溶剂50-300份。
进一步的,所述混合胶液的固含量为25-30%;涂布胶膜厚度为10-50μm。
进一步的,所述气相二氧化硅为AEROSIL@气相法二氧化硅中的至少一种;所述无卤阻燃剂为亚膦酸盐阻燃剂、二乙基次磷酸铝氢氧化铝、有机硅阻燃剂FRX-210、三聚氰胺氰尿酸盐脂的至少一种;所述环氧树脂为双酚A型高分子量热塑性环氧树脂;所述环氧酚醛树脂为多官能团酚醛环氧树脂,环氧当量170-180;所述溶剂为丁酮、乙酸乙酯、甲苯、异丙醇中的至少一种。
与现有技术相比,本发明所达到的有益效果是:本发明制备两种中温固化剂:改性异氰酸酯A与B,并按照一定的比例与高温固化剂二氨基二苯砜混合得到复合固化剂,一方面改善了单一固化剂的缺点,降低了压合温度并提高了对金属材料的粘接力,同时改性异氰酸酯能够增韧环氧树脂改善了固化后胶膜脆的缺点。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
以下实施例中,二氨基二苯砜由中国阿拉丁试剂公司提供,分析纯;气相二氧化硅由卡博特有限公司提供,型号为TS720;无卤阻燃剂由科莱恩化工有限公司提供,型号为OP935;环氧树脂由沈阳沃丰达科技有限公司提供,环氧当量250-400;环氧酚醛树脂由上海丰觉化工有限公司提供,环氧当量170-180;芳香族异氰酸酯由上海麦克林生化科技股份有限公司提供。
实施例1
S1:按照质量比1∶7∶2依次将改性多异氰酸酯A,改性多异氰酸酯B,二氨基二苯砜加入到溶剂中,混合均匀,得到复合固化剂;
S2:将1份气相二氧化硅、25份无卤阻燃剂均匀分散在50份环氧树脂中,并依次加入15份环氧酚醛树脂、5份复合固化剂和150份甲苯,混合均匀,得到混合胶液;涂布于薄膜上,厚度为50μm,烘干,得到叠层母排用绝缘阻燃胶膜。
实施例2
S1:按照质量比2∶5∶3依次将改性多异氰酸酯A,改性多异氰酸酯B,二氨基二苯砜加入到溶剂中,混合均匀,得到复合固化剂;
S2:将1.5份气相二氧化硅、20份无卤阻燃剂均匀分散在45份环氧树脂中,并依次加入10份环氧酚醛树脂、10份复合固化剂和150份丁酮,混合均匀,得到混合胶液;涂布于薄膜上,厚度为50μm,烘干,得到叠层母排用绝缘阻燃胶膜。
实施例3
S1:按照质量比3∶3∶4依次将改性多异氰酸酯A,改性多异氰酸酯B,二氨基二苯砜加入到溶剂中,混合均匀,得到复合固化剂;
S2:将1.5份气相二氧化硅、20份无卤阻燃剂均匀分散在45份环氧树脂中,并依次加入10份环氧酚醛树脂、15份复合固化剂和150份丁酮,混合均匀,得到混合胶液;涂布于薄膜上,厚度为50μm,烘干,得到叠层母排用绝缘阻燃胶膜。
对比例1
将1.5份气相二氧化硅、20份无卤阻燃剂均匀分散在45份环氧树脂中,并依次加入10份环氧酚醛树脂、10份改性多异氰酸酯A和150份甲苯,混合均匀,得到混合胶液;涂布于薄膜上,厚度为50μm,烘干,得到叠层母排用绝缘阻燃胶膜。
对比例2
将1.5份气相二氧化硅、20份无卤阻燃剂均匀分散在45份环氧树脂中,并依次加入10份环氧酚醛树脂、10份改性多异氰酸酯B和150份丁酮,混合均匀,得到混合胶液;涂布于薄膜上,厚度为50μm,烘干,得到叠层母排用绝缘阻燃胶膜。
对比例3
将1份气相二氧化硅、25份无卤阻燃剂均匀分散在50份环氧树脂中,并依次加入15份环氧酚醛树脂、5份二氨基二苯砜和150份丁酮,混合均匀,得到混合胶液;涂布于薄膜上,厚度为50μm,烘干,得到叠层母排用绝缘阻燃胶膜。
测试方法:
1、按照ASTM D3330测试绝缘胶膜与铜箔的粘结力,180°剥离试验,;
2、冷热冲击性能,将绝缘胶膜与铜排高温压合,然后进行冷热冲击试验。冷热冲击试验条件为:-40℃~130℃/1000次循环,-40℃/恒温2小时,-040℃升温至130℃/1分钟,130℃/恒温2小时,130℃降温至-40℃/1分钟,以上一个循环约为4小时。冷热冲击后胶膜与铜板之间无气泡、无开裂则为合格,否则不合格。
3、湿热老化性能,将绝缘胶膜与铜排高温压合,然后进行湿热老化试验。湿热老化试验条件为:85℃×85%RH/2000小时。湿热老化后胶膜与铜排间无气泡、脱层、开裂则为合格,否则不合格。
4、加工性(折弯测试),将厚度为3mm的铜排与胶膜高温压合后冷却至室温,进行折弯试验,弯折角度为150°。
5、阻燃性,依据UL 94垂直燃烧法测定。
6、电气强度,绝缘胶膜连接设备后,加电压,频率为50Hz,计算击穿时的电气强度。
测试数据见下表。
结论:实施例3制备得到的胶膜具有优异的电气强度及各项性能;对比例1-3中,分别加入了改性多异氰酸酯A,改性多异氰酸酯B和二氨基二苯砜替代了实施例中的复合固化剂制备得到的胶膜性能较差。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:包括以下步骤:
S1:将改性多异氰酸酯和二氨基二苯砜加入到溶剂中,混合均匀,得到复合固化剂;
S2:将气相二氧化硅、无卤阻燃剂均匀分散在环氧树脂中,并依次加入环氧酚醛树脂、复合固化剂和溶剂,混合均匀,得到混合胶液;涂布于薄膜上,烘干,得到叠层母排用绝缘阻燃胶膜。
2.根据权利要求1所述的叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:步骤S1中,改性多异氰酸酯∶二氨基二苯砜的质量比为1∶1-4∶1;其中,所述改性多异氰酸酯为改性多异氰酸酯A和改性多异氰酸酯B的混合物,改性多异氰酸酯A∶改性多异氰酸酯B的质量比为1∶9-9∶1。
3.根据权利要求1所述的叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:步骤S1中,所述溶剂为丁酮、乙酸乙酯、甲苯或异丙醇中的至少一种。
4.根据权利要求2所述的叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:所述改性多异氰酸酯A为端羟基聚丙烯酸甲酯-丙烯酸丁酯与芳香族异氰酸酯制备得到。
5.根据权利要求2所述的叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:所述改性多异氰酸酯B为聚酯与芳香族异氰酸酯制备得到。
6.根据权利要求1所述的叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:叠层母排用绝缘阻燃胶膜中,按质量份数计,包括以下组分:
复合固化剂5-15份,气相二氧化硅0.1-3份,无卤素阻燃剂20-30份,环氧树脂10-50份,环氧酚醛树脂5-25份,溶剂50-300份。
7.根据权利要求1所述的叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:步骤S2中,所述混合胶液的固含量为25-30%;涂布胶膜厚度为10-50μm。
8.根据权利要求1所述的叠层母排用绝缘阻燃胶膜的制备方法,其特征在于:步骤S2中,所述无卤阻燃剂为亚膦酸盐阻燃剂、二乙基次磷酸铝、氢氧化铝、有机硅阻燃剂FRX-210、三聚氰胺氰尿酸盐脂的至少一种;所述环氧树脂环氧当量250-400;所述环氧酚醛树脂环氧当量为170-180;所述溶剂为丁酮、乙酸乙酯、甲苯、异丙醇中的至少一种。
9.根据权利要求1-8任一项所述的叠层母排用绝缘阻燃胶膜的制备方法制备得到的绝缘阻燃胶膜。
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