CN110563988B - 一种耐高温聚酰亚胺/聚四氟乙烯抗粘结复合膜及其制备方法 - Google Patents

一种耐高温聚酰亚胺/聚四氟乙烯抗粘结复合膜及其制备方法 Download PDF

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CN110563988B
CN110563988B CN201910898965.XA CN201910898965A CN110563988B CN 110563988 B CN110563988 B CN 110563988B CN 201910898965 A CN201910898965 A CN 201910898965A CN 110563988 B CN110563988 B CN 110563988B
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李辉
周翠平
赵绚
刘双双
胡明爽
刘釜铭
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Abstract

本发明提供一种耐高温聚酰亚胺/聚四氟乙烯抗粘结复合膜及其制备方法，将润滑油均匀的刷涂在经等离子体处理的含氟聚酰亚胺/聚四氟乙烯薄膜表面上，得到抗粘结复合膜复合膜。同时提供了等离子体处理含氟聚酰亚胺/聚四氟乙烯薄膜的方法，该方法成本低、无废弃物、无污染、工艺简单、技术要求低、生产可控性强，吸附润滑油后具有良好的绝缘、抗粘附、抗静电、高低温、耐腐蚀等特性。

Description

一种耐高温聚酰亚胺/聚四氟乙烯抗粘结复合膜及其制备 方法
技术领域
本发明涉及一种耐高温含氟聚酰亚胺/聚四氟乙烯抗粘结复合膜及其制备方法，属于复合膜材料制备领域。
背景技术
聚酰亚胺材料凭借优异的耐高低温，耐热，耐化学品，绝缘，抗粘等性能，在导电带、航空航天领域中的电磁屏蔽外罩、化工和军工用的防静电服、防尘服等方面应用广泛。但是现有的工业化聚酰亚胺复合膜最高使用温度仅为260℃，并且在高温下长时间使用会出现表面粘结现象。在聚酰亚胺复合膜中引入含氟组分，在高温下，氟元素向表面迁移，使得膜材料表面能降低，耐腐蚀、耐高低温及绝缘性能提高，此外在表面涂覆润滑油有助于改善聚酰亚胺膜材料的耐温性及抗粘性，拓宽其应用范围，为聚酰亚胺薄膜材料的研究及应用提供了新方向。
发明内容
为了解决上述问题，本发明提供一种耐高温含氟聚酰亚胺/聚四氟乙烯抗粘结复合膜及其制备方法，其制备方法成本低、无废弃物、无污染、工艺简单、技术要求低、生产可控性强，吸附润滑油后具有良好的绝缘、抗粘附、抗静电、耐高低温、耐腐蚀、绝缘、润滑等特性。
本发明是通过以下技术方案实现的：
一种耐高温聚酰亚胺/聚四氟乙烯抗粘结复合膜，其特征在于，是由具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜与润滑油构成。
上述的高温聚酰亚胺/聚四氟乙烯抗粘结复合膜的制备方法，其特征在于，将润滑油均匀的刷涂在具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜上，静置3-24h后，得到复合膜。
上述的润滑油为全氟聚醚、全氟三戊胺、全氟三丁胺和硅油中的一种或其混合物，刷涂量为0.2-1.0L/m2。
上述的具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜的制备方法为：将含氟聚酰亚胺/聚四氟乙烯薄膜放入无水乙醇中浸泡10min，取出后在滤纸表面晾干，然后将处理后的含氟聚酰亚胺/聚四氟乙烯薄膜放入设定电压的等离子体多功能实验台的反应室，在不同惰性气体及一定工作压力下，进行等离子体表面处理得到具有拓扑结构的改性含氟聚酰亚胺/聚四氟乙烯薄膜。
上述的设定电压为500～600V，惰性气体为氮气、氩气、氦气中的一种或两种的混合物，工作压力为10~1000Pa，处理时间为5 min~ 60min。
上述的含氟聚酰亚胺/聚四氟乙烯复合膜是含氟聚酰亚胺和聚四氟乙烯是通过流延法制备而成，其厚度为5～300μm。
上述的聚四氟乙烯粉末的粒径为500-2000nm。
上述的含氟聚酰亚胺，其结构如式Ⅰ所示：
Figure 450451DEST_PATH_IMAGE002
。
上述的含氟聚酰亚胺/聚四氟乙烯薄膜的拉伸强度为100～150MPa，断裂伸长率为20～150%，弹性模量为（1000～3000MPa）。
上述所述的制备方法制备的含氟聚酰亚胺/聚四氟乙烯抗粘结复合膜，水接触角大于100°，接触角滞后低于20°，介电常数低于5，介电损耗低于0.008，耐受温度为200-350℃。
有益效果
本发明的含氟聚酰亚胺/聚四氟乙烯复合膜是由具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜与润滑油通过吸附作用复合而成。其中含氟聚酰亚胺/聚四氟乙烯薄膜具有优异的力学性能，拉伸强度为100～150MPa，断裂伸长率为20～150%，弹性模量为1000～3000MPa，制备的复合膜水接触角大于100°，接触角滞后低于20°，并且润滑油的存在使得复合膜具有良好的绝缘、抗粘附、抗静电、高低温、耐腐蚀性等特点，介电常数低于7，介电损耗低于0.008，耐受温度为200-350℃。可在绝缘、防覆冰、抗粘附等领域应用。
附图说明
图1是本发明中含氟聚酰亚胺的结构简式。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1
制备含氟聚酰亚胺/聚四氟乙烯薄膜，制备方法为：将含氟聚酰胺酸溶液（质量分数70%）与聚四氟乙烯粉末（分子量10000g/mol，质量分数30%）共混得到混合溶液，将溶液在干燥、光滑且洁净的玻璃板上均匀流延，干燥温度为280℃，干燥时间为3min；烧结分两阶段：室温加热至120℃，保温5min，升温速率为10℃/min；升温至330℃，保温3min，升温速率为15℃/min，得含氟聚酰亚胺/聚四氟乙烯薄膜。
制备具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜，制备方法为：将尺寸为50mm×50mm×10μm的含氟聚酰亚胺/聚四氟乙烯薄膜经乙醇预处理后，置于500V电压的等离子体多功能实验台的反应室中，在氮气氛围下，设置工作压力为30Pa，处理60分钟得到表面改性的含氟聚酰亚胺/聚四氟乙烯薄膜。
制备抗粘结复合膜：将全氟聚醚（40mm2/s，刷涂量为0.2L/m2）均匀的涂刷在具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜上，静置24小时，得到含氟聚酰亚胺/聚四氟乙烯薄膜复合膜。
实施例2
制备含氟聚酰亚胺/聚四氟乙烯薄膜，制备方法为：以4,4' -(六氟异丙烯)二酞酸酐与4,4' -二胺基二苯醚为原料通过缩聚反应合成含氟聚酰胺酸。将含氟聚酰胺酸溶液（质量分数50%）与聚四氟乙烯粉末（分子量20000g/mol，质量分数50%）共混得到混合溶液，将溶液在干燥、光滑且洁净的玻璃板上均匀流延，干燥温度为250℃，干燥时间为5min；烧结分两阶段：室温加热至120℃，保温5min，升温速率为10℃/min；升温至310℃，保温3min，升温速率为15℃/min，得含氟聚酰亚胺/聚四氟乙烯薄膜。
制备具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜，制备方法为：将尺寸为50mm×50mm×20μm的含氟聚酰亚胺/聚四氟乙烯薄膜经乙醇预处理后，置于500V电压的等离子体多功能实验台的反应室中，在氩气氛围下，设置工作压力为50Pa，处理30分钟得到表面改性的含氟聚酰亚胺/聚四氟乙烯薄膜。
制备抗粘结复合膜：将全氟三戊胺（刷涂量为0.7L/m2）均匀的涂刷在具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜上，静置3小时，得到复合膜。
实施例3
制备含氟聚酰亚胺/聚四氟乙烯薄膜，制备方法为：以4,4' -(六氟异丙烯)二酞酸酐与4,4' -二胺基二苯醚为原料通过缩聚反应合成含氟聚酰胺酸。将含氟聚酰胺酸溶液（质量分数30%）与聚四氟乙烯粉末（分子量30000g/mol，质量分数70%）共混得到混合溶液，将溶液在干燥、光滑且洁净的玻璃板上均匀流延，干燥温度为220℃，干燥时间为10min；烧结分两阶段：室温加热至120℃，保温5min，升温速率为10℃/min；升温至280℃，保温3min，升温速率为15℃/min，得含氟聚酰亚胺/聚四氟乙烯薄膜。
制备具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜，制备方法为：将尺寸为50mm×50mm×20μm的含氟聚酰亚胺薄膜经乙醇预处理后，置于500V电压的等离子体多功能实验台的反应室中，在氦气氛围下，设置工作压力为100Pa，处理5分钟得到表面改性的含氟聚酰亚胺薄膜。
制备抗粘结复合膜：将硅油（10mPa/s，刷涂量为1.0L/m2）均匀的涂刷在具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜上，静置15小时，得到复合膜。
实施例1-3所制备的含氟聚酰亚胺/聚四氟乙烯复合膜的力学、耐温性及介电性能如表1所示：
表1 含氟聚酰亚胺/聚四氟乙烯复合膜的力学、耐温性及介电性能
Figure 811332DEST_PATH_IMAGE004
本发明制备的含氟聚酰亚胺/聚四氟乙烯复合膜与现有的聚酰亚胺复合膜相比较，本发明复合膜拉伸强度为100～150MPa，断裂伸长率为20～150%，弹性模量为1000～3000MPa，水接触角大于100°，接触角滞后低于20°，介电常数低于5，介电损耗低于0.008，耐受温度为200-350℃。
显然，本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样，倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内，则本发明也意图包含这些改动和变型在内。

Claims (5)

1.一种耐高温聚酰亚胺/聚四氟乙烯抗粘结复合膜，其特征在于，是由具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜吸附润滑油构成，
所述的含氟聚酰亚胺/聚四氟乙烯薄膜是含氟聚酰亚胺和聚四氟乙烯通过流延法制备而成，其厚度为5～300μm，
所述的含氟聚酰亚胺，其结构如式Ⅰ所示：
Figure FDA0003458300820000011
所述的聚四氟乙烯为粒径范围处于500nm～2000nm的粉末，
所述的润滑油为全氟聚醚、全氟三戊胺、全氟三丁胺和硅油中的一种或其混合物，刷涂量为0.2～1.0L/m2。
2.一种权利要求1所述的耐高温聚酰亚胺/聚四氟乙烯抗粘结复合膜的制备方法，其特征在于，将润滑油均匀的刷涂在具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜上，静置3～24h后，得到复合膜。
3.根据权利要求2所述的制备方法，其特征在于，所述的具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜的制备方法为：将含氟聚酰亚胺/聚四氟乙烯薄膜放入无水乙醇中浸泡10min，取出后在滤纸表面晾干，然后将处理后的含氟聚酰亚胺/聚四氟乙烯薄膜放入设定为500～600V电压的等离子体多功能实验台的反应室，在氮气、氩气或氦气惰性气体条件及处于10～1000Pa的工作压力下，进行1min～60min的等离子体表面处理得到具有拓扑结构的含氟聚酰亚胺/聚四氟乙烯薄膜。
4.根据权利要求2所述的制备方法，其特征在于，所述的含氟聚酰亚胺/聚四氟乙烯复合膜的拉伸强度为100～150MPa，断裂伸长率为20～150％。
5.根据权利要求2所述的制备方法制备的含氟聚酰亚胺/聚四氟乙烯抗粘附复合膜水接触角大于100°，接触角滞后低于20°，介电常数低于5，耐受温度为200～350℃。
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