CN109591411A - 一种聚酰亚胺厚板的制备方法 - Google Patents

一种聚酰亚胺厚板的制备方法 Download PDF

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CN109591411A
CN109591411A CN201811421958.2A CN201811421958A CN109591411A CN 109591411 A CN109591411 A CN 109591411A CN 201811421958 A CN201811421958 A CN 201811421958A CN 109591411 A CN109591411 A CN 109591411A
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岑建军
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NINGBO JINSHAN NEW MATERIAL Co.,Ltd.
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Abstract

本发明公开了一种聚酰亚胺厚板的制备方法，其通过将热固性聚酰亚胺和热塑性聚酰亚胺叠加而得到的聚酰亚胺厚板，厚度从300微米到1000微米，没有使用环氧树脂或者丙烯酸树脂等非聚酰亚胺物质。本发明得到的聚酰亚胺厚板的表面平整，光滑，粘结力大于10N/mm，不分层。

Description

一种聚酰亚胺厚板的制备方法
技术领域
本发明涉及一种聚酰亚胺板，特别是一种聚酰亚胺厚板的制备方法。
背景技术
聚酰亚胺由于具有优异的耐热性和机械特性，因此正被广泛应用于各种工业领域。但是一般聚酰亚胺薄膜的最厚厚度只有250微米，再厚就难以制作。
发明内容
本发明的目的是为了解决上述现有技术的不足而提供一种聚酰亚胺厚板的制备方法。
为了实现上述目的，本发明所设计的一种聚酰亚胺厚板的制备方法，包括以下步骤：
步骤一、制备热固性聚酰亚胺薄膜，先将二胺放入反应釜中，并用极性溶剂溶解，然后放入改性纳米粉末，最后再分批加入二酐到反应釜中，搅拌，最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP，再脱泡流延成膜即可得到热固性聚酰亚胺薄膜；其中改性纳米粉末按重量份包括20-30份四氟化硅、10-15份氧化铝、30-40份氧化硅、1-5份氧化钛、0.1-0.3份氧化铪；
步骤二、涂覆热塑性聚酰亚胺，在上述得到的热固性聚酰亚胺薄膜上涂上一层热塑性聚酰亚胺，涂层厚度在3-7微米，具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面，接着放置到设置有烘箱的传送带上，完成聚酰胺酸的彻底亚胺化，其中烘箱的梯次温度为80-380℃，传送带的速度2-15米/min；
步骤三、制备聚酰亚胺厚板，根据所需厚度的聚酰亚胺厚板，将已经涂好热塑性聚酰亚胺薄膜的热固性聚酰亚胺薄膜叠压起来，每层必须依次热固性与热塑性接合，最外面的上下两层均为热固性聚酰亚胺薄膜，然后放入500℃的高温真空压机内，升温加压，温度升到300-350度之间，压力升到不小于6kgf/平方厘米，停留保温时间在3-10分钟即可降温，降到100以下时可开机取出厚板。
所述烘箱的梯次温度具体为
从80℃加热至100℃，保温30-60min，
加热升温至160℃，保温15-30min，
加热升温至200℃，保温15-30min，
加热升温至250℃，保温30-60min，
加热升温至300℃，保温15-30min，
加热升温至380℃，保温5-15min。
所述二酐为均苯四甲酸二酐（PMDA）、3,3',4,4'-联苯四羧酸二酐（BPDA）、3,3',4,4'-二苯酮四酸二酐(BTDA)、4,4'-联苯醚二酐(ODPA)、双酚A二酐（BPADA）、4,4'-(六氟异丙烯)二酞酸酐(6FPA)中的一种或几种；
所述二胺为4,4-二氨基二苯醚（ODA）、对苯二胺（PPD）、4,4-二氨基二苯基甲烷（MDA）、2,2'-双(三氟甲基)-4,4'-二氨基联苯(TFMB)（TFMB）、4,4-二氨基苯砜（4,4-DDS）、1,4-双(4-氨基-2-三氟甲基苯氧基)苯（6FAPB）中的一种或几种；
所述的极性溶剂是二甲基乙酰胺（DMAC）、N-甲基吡咯烷酮（NMP）、二甲基甲酰胺（DMF）中的一种或几种。
本发明得到的一种聚酰亚胺厚板的制备方法，其通过将热固性聚酰亚胺和热塑性聚酰亚胺叠加而得到的聚酰亚胺厚板，厚度从300微米到1000微米，没有使用环氧树脂或者丙烯酸树脂等非聚酰亚胺物质。且聚酰亚胺厚板的表面平整，光滑，粘结力大于10N/mm，不分层。
具体实施方式
下面结合实施例对本发明进一步说明。
实施例1：
本实施例提供的一种聚酰亚胺厚板的制备方法，包括以下步骤：
步骤一、制备热固性聚酰亚胺薄膜，先将二胺放入反应釜中，并用极性溶剂溶解，然后放入改性纳米粉末，最后再分批加入二酐到反应釜中，搅拌，最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP，再脱泡流延成膜即可得到热固性聚酰亚胺薄膜；其中改性纳米粉末按重量份包括20份四氟化硅、10份氧化铝、30份氧化硅、1份氧化钛、0.1份氧化铪；
步骤二、涂覆热塑性聚酰亚胺，在上述得到的热固性聚酰亚胺薄膜上涂上一层热塑性聚酰亚胺，涂层厚度在3-7微米，具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面，接着放置到设置有烘箱的传送带上，完成聚酰胺酸的彻底亚胺化，其中烘箱的梯次温度为80-380℃，传送带的速度2-15米/min；
步骤三、制备聚酰亚胺厚板，根据所需厚度的聚酰亚胺厚板，将已经涂好热塑性聚酰亚胺薄膜的热固性聚酰亚胺薄膜叠压起来，每层必须依次热固性与热塑性接合，最外面的上下两层均为热固性聚酰亚胺薄膜，然后放入500℃的高温真空压机内，升温加压，温度升到300-350度之间，压力升到不小于6kgf/平方厘米，停留保温时间在3-10分钟即可降温，降到100以下时可开机取出厚板。
所述烘箱的梯次温度具体为
从80℃加热至100℃，保温30-60min，
加热升温至160℃，保温15-30min，
加热升温至200℃，保温15-30min，
加热升温至250℃，保温30-60min，
加热升温至300℃，保温15-30min，
加热升温至380℃，保温5-15min。
所述二酐为均苯四甲酸二酐（PMDA）、3,3',4,4'-联苯四羧酸二酐（BPDA）、3,3',4,4'-二苯酮四酸二酐(BTDA)、4,4'-联苯醚二酐(ODPA)、双酚A二酐（BPADA）、4,4'-(六氟异丙烯)二酞酸酐(6FPA)中的一种或几种；
所述二胺为4,4-二氨基二苯醚（ODA）、对苯二胺（PPD）、4,4-二氨基二苯基甲烷（MDA）、2,2'-双(三氟甲基)-4,4'-二氨基联苯(TFMB)（TFMB）、4,4-二氨基苯砜（4,4-DDS）、1,4-双(4-氨基-2-三氟甲基苯氧基)苯（6FAPB）中的一种或几种；
所述的极性溶剂是二甲基乙酰胺（DMAC）、N-甲基吡咯烷酮（NMP）、二甲基甲酰胺（DMF）中的一种或几种。
实施例2：
本实施例提供的一种聚酰亚胺厚板的制备方法，包括以下步骤：
步骤一、制备热固性聚酰亚胺薄膜，先将二胺放入反应釜中，并用极性溶剂溶解，然后放入改性纳米粉末，最后再分批加入二酐到反应釜中，搅拌，最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP，再脱泡流延成膜即可得到热固性聚酰亚胺薄膜；其中改性纳米粉末按重量份包括30份四氟化硅、15份氧化铝、40份氧化硅、5份氧化钛、0.3份氧化铪；
步骤二、涂覆热塑性聚酰亚胺，在上述得到的热固性聚酰亚胺薄膜上涂上一层热塑性聚酰亚胺，涂层厚度在3-7微米，具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面，接着放置到设置有烘箱的传送带上，完成聚酰胺酸的彻底亚胺化，其中烘箱的梯次温度为80-380℃，传送带的速度2-15米/min；
步骤三、制备聚酰亚胺厚板，根据所需厚度的聚酰亚胺厚板，将已经涂好热塑性聚酰亚胺薄膜的热固性聚酰亚胺薄膜叠压起来，每层必须依次热固性与热塑性接合，最外面的上下两层均为热固性聚酰亚胺薄膜，然后放入500℃的高温真空压机内，升温加压，温度升到300-350度之间，压力升到不小于6kgf/平方厘米，停留保温时间在3-10分钟即可降温，降到100以下时可开机取出厚板。
实施例3：
本实施例提供的一种聚酰亚胺厚板的制备方法，包括以下步骤：
步骤一、制备热固性聚酰亚胺薄膜，先将二胺放入反应釜中，并用极性溶剂溶解，然后放入改性纳米粉末，最后再分批加入二酐到反应釜中，搅拌，最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP，再脱泡流延成膜即可得到热固性聚酰亚胺薄膜；其中改性纳米粉末按重量份包括25份四氟化硅、12份氧化铝、35份氧化硅、3份氧化钛、0.2份氧化铪；
步骤二、涂覆热塑性聚酰亚胺，在上述得到的热固性聚酰亚胺薄膜上涂上一层热塑性聚酰亚胺，涂层厚度在3-7微米，具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面，接着放置到设置有烘箱的传送带上，完成聚酰胺酸的彻底亚胺化，其中烘箱的梯次温度为80-380℃，传送带的速度2-15米/min；
步骤三、制备聚酰亚胺厚板，根据所需厚度的聚酰亚胺厚板，将已经涂好热塑性聚酰亚胺薄膜的热固性聚酰亚胺薄膜叠压起来，每层必须依次热固性与热塑性接合，最外面的上下两层均为热固性聚酰亚胺薄膜，然后放入500℃的高温真空压机内，升温加压，温度升到300-350度之间，压力升到不小于6kgf/平方厘米，停留保温时间在3-10分钟即可降温，降到100以下时可开机取出厚板。

Claims (3)

1.一种聚酰亚胺厚板的制备方法，其特征在于：包括以下步骤：
步骤一、制备热固性聚酰亚胺薄膜，先将二胺放入反应釜中，并用极性溶剂溶解，然后放入改性纳米粉末，最后再分批加入二酐到反应釜中，搅拌，最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP，再脱泡流延成膜即可得到热固性聚酰亚胺薄膜；其中改性纳米粉末按重量份包括20-30份四氟化硅、10-15份氧化铝、30-40份氧化硅、1-5份氧化钛、0.1-0.3份氧化铪；
步骤二、涂覆热塑性聚酰亚胺，在上述得到的热固性聚酰亚胺薄膜上涂上一层热塑性聚酰亚胺，涂层厚度在3-7微米，具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面，接着放置到设置有烘箱的传送带上，完成聚酰胺酸的彻底亚胺化，其中烘箱的梯次温度为80-380℃，传送带的速度2-15米/min；
步骤三、制备聚酰亚胺厚板，根据所需厚度的聚酰亚胺厚板，将已经涂好热塑性聚酰亚胺薄膜的热固性聚酰亚胺薄膜叠压起来，每层必须依次热固性与热塑性接合，最外面的上下两层均为热固性聚酰亚胺薄膜，然后放入500℃的高温真空压机内，升温加压，温度升到300-350度之间，压力升到不小于6kgf/平方厘米，停留保温时间在3-10分钟即可降温，降到100以下时可开机取出厚板。
2.根据权利要求1所述的一种聚酰亚胺厚板的制备方法，其特征在于：所述二酐为均苯四甲酸二酐（PMDA）、3,3',4,4'-联苯四羧酸二酐（BPDA）、3,3',4,4'-二苯酮四酸二酐(BTDA)、4,4'-联苯醚二酐(ODPA)、双酚A二酐（BPADA）、4,4'-(六氟异丙烯)二酞酸酐(6FPA)中的一种或几种；
所述二胺为4,4-二氨基二苯醚（ODA）、对苯二胺（PPD）、4,4-二氨基二苯基甲烷（MDA）、2,2'-双(三氟甲基)-4,4'-二氨基联苯(TFMB)（TFMB）、4,4-二氨基苯砜（4,4-DDS）、1,4-双(4-氨基-2-三氟甲基苯氧基)苯（6FAPB）中的一种或几种；
所述的极性溶剂是二甲基乙酰胺（DMAC）、N-甲基吡咯烷酮（NMP）、二甲基甲酰胺（DMF）中的一种或几种。
3.根据权利要求1所述的一种聚酰亚胺厚板的制备方法，其特征在于：
所述烘箱的梯次温度具体为
从80℃加热至100℃，保温30-60min，
加热升温至160℃，保温15-30min，
加热升温至200℃，保温15-30min，
加热升温至250℃，保温30-60min，
加热升温至300℃，保温15-30min，
加热升温至380℃，保温5-15min。
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