CN110437614A - 可成型聚酰亚胺薄膜的制备方法 - Google Patents
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Abstract
本发明公开了可成型聚酰亚胺薄膜的制备方法,先将两种二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米填料和增塑剂,最后再分批加入两种二酐到反应釜中,搅拌,制备成所需的聚酰胺酸溶液;接着将上述混合均匀的聚酰胺酸溶液经过真空脱泡后流延至钢带或者玻璃基材上,并在干燥惰性气体的保护下采用远红外加热的方式经拉伸亚胺化得到聚酰亚胺薄膜。本发明得到的可成型聚酰亚胺薄膜的制备方法得到的可成型聚酰亚胺薄膜,厚度在25um~125um,最佳成型温度为350℃。成型后不会变形,同时能保持薄膜本身良好的物理、电气和机械性能。
Description
技术领域
本发明涉及一种聚酰亚胺薄膜,特别是可成型聚酰亚胺薄膜的制备方法。
背景技术
聚酰亚胺薄膜(PI)是指主链上含有酰亚胺环的一类聚合物,具有优异的机械性能、耐高低温性能和耐辐射性能,并且其电阻率高、介电常数低,因而作为保护覆盖膜和基材已广泛应用于航空航天、微电子行业等领域。但是目前国内的聚酰亚胺薄膜与国外的相比,仍存在较大差距,具体体现在拉伸强度低,尺寸稳定性差,成型后容易变形。
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成型后不会变形的可成型聚酰亚胺薄膜的制备方法。
为了实现上述目的,本发明所设计的可成型聚酰亚胺薄膜的制备方法,包括以下步骤:
步骤一、制备聚酰胺酸溶液,先将两种二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米填料和增塑剂,最后再分批加入两种二酐到反应釜中,搅拌,制备成所需的聚酰胺酸溶液;其中改性纳米填料和增塑剂占聚酰胺酸溶液的质量比分别为2%和1%;所述改性纳米填料按重量份包括20-30份碳纤维、40-50份二氧化硅、10-15份四氟化硅以及5-10份碳化硅;
步骤二、制备可成型聚酰亚胺薄膜,将上述混合均匀的聚酰胺酸溶液经过真空脱泡后流延至钢带或者玻璃基材上,并在干燥惰性气体的保护下采用远红外加热的方式,具体是先在100-120℃保持10-20min,然后依次在140-160℃保持10-20min,在180-220℃保持10-20min,在220-280℃保持10-20min,在320-380℃保持10-20min,在380-400℃保持5-10min,经拉伸亚胺化得到聚酰亚胺薄膜。
所述增塑剂为增塑剂选自邻苯二甲酸二辛脂(DOP)、邻苯二甲酸二丁脂(DBP)、过氧化二异丙苯(DCP)和邻苯二甲酸二乙脂(DEP)中的一种或几种。
所述制备聚酰胺酸溶液中的二酐为均苯四甲酸二酐(PMDA)、氢化均苯四甲酸二酐(HPMDA)、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)中的两种或几种;
所述二胺为4,4-二氨基二苯醚(4,4-ODA)、3,4’-二氨基二苯醚(3,4-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)、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)、1,3-二(4-氨基苯氧基)苯(1,3,4-APB)中的两种或几种;
所述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。
本发明得到的可成型聚酰亚胺薄膜的制备方法得到的可成型聚酰亚胺薄膜,厚度在25um~125um,最佳成型温度为350℃。成型后不会变形,同时能保持薄膜本身良好的物理、电气和机械性能。
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:
本实施例提供的可成型聚酰亚胺薄膜的制备方法,包括以下步骤:
步骤一、制备聚酰胺酸溶液,先将两种二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米填料和增塑剂,最后再分批加入两种二酐到反应釜中,搅拌,制备成所需的聚酰胺酸溶液;其中改性纳米填料和增塑剂占聚酰胺酸溶液的质量比分别为2%和1%;所述改性纳米填料按重量份包括20份碳纤维、40份二氧化硅、10份四氟化硅以及5份碳化硅;
步骤二、制备可成型聚酰亚胺薄膜,将上述混合均匀的聚酰胺酸溶液经过真空脱泡后流延至钢带或者玻璃基材上,并在干燥惰性气体的保护下采用远红外加热的方式,具体是先在100-120℃保持10-20min,然后依次在140-160℃保持10-20min,在180-220℃保持10-20min,在220-280℃保持10-20min,在320-380℃保持10-20min,在380-400℃保持5-10min,经拉伸亚胺化得到聚酰亚胺薄膜。
所述增塑剂为增塑剂选自邻苯二甲酸二辛脂(DOP)、邻苯二甲酸二丁脂(DBP)、过氧化二异丙苯(DCP)和邻苯二甲酸二乙脂(DEP)中的一种或几种。
所述制备聚酰胺酸溶液中的二酐为均苯四甲酸二酐(PMDA)、氢化均苯四甲酸二酐(HPMDA)、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)中的两种或几种;
所述二胺为4,4-二氨基二苯醚(4,4-ODA)、3,4’-二氨基二苯醚(3,4-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)、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)、1,3-二(4-氨基苯氧基)苯(1,3,4-APB)中的两种或几种;
所述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。
经测试,本实施例得到的可成型聚酰亚胺薄膜,其横向断裂伸长率大于26%,纵向断裂伸长率大于120%。
实施例2:
本实施例提供的可成型聚酰亚胺薄膜的制备方法,包括以下步骤:
步骤一、制备聚酰胺酸溶液,先将两种二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米填料和增塑剂,最后再分批加入两种二酐到反应釜中,搅拌,制备成所需的聚酰胺酸溶液;其中改性纳米填料和增塑剂占聚酰胺酸溶液的质量比分别为2%和1%;所述改性纳米填料按重量份包括30份碳纤维、50份二氧化硅、15份四氟化硅以及10份碳化硅;
步骤二、制备可成型聚酰亚胺薄膜,将上述混合均匀的聚酰胺酸溶液经过真空脱泡后流延至钢带或者玻璃基材上,并在干燥惰性气体的保护下采用远红外加热的方式,具体是先在100-120℃保持10-20min,然后依次在140-160℃保持10-20min,在180-220℃保持10-20min,在220-280℃保持10-20min,在320-380℃保持10-20min,在380-400℃保持5-10min,经拉伸亚胺化得到聚酰亚胺薄膜。
经测试,本实施例得到的可成型聚酰亚胺薄膜,其横向断裂伸长率大于26%,纵向断裂伸长率大于120%。
实施例3:
本实施例提供的可成型聚酰亚胺薄膜的制备方法,包括以下步骤:
步骤一、制备聚酰胺酸溶液,先将两种二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米填料和增塑剂,最后再分批加入两种二酐到反应釜中,搅拌,制备成所需的聚酰胺酸溶液;其中改性纳米填料和增塑剂占聚酰胺酸溶液的质量比分别为2%和1%;所述改性纳米填料按重量份包括25份碳纤维、45份二氧化硅、15份四氟化硅以及8份碳化硅;
步骤二、制备可成型聚酰亚胺薄膜,将上述混合均匀的聚酰胺酸溶液经过真空脱泡后流延至钢带或者玻璃基材上,并在干燥惰性气体的保护下采用远红外加热的方式,具体是先在100-120℃保持10-20min,然后依次在140-160℃保持10-20min,在180-220℃保持10-20min,在220-280℃保持10-20min,在320-380℃保持10-20min,在380-400℃保持5-10min,经拉伸亚胺化得到聚酰亚胺薄膜。
经测试,本实施例得到的可成型聚酰亚胺薄膜,其横向断裂伸长率大于26%,纵向断裂伸长率大于120%。
Claims (5)
1.一种可成型聚酰亚胺薄膜的制备方法,其特征在于:包括以下步骤:
步骤一、制备聚酰胺酸溶液,先将两种二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米填料和增塑剂,最后再分批加入两种二酐到反应釜中,搅拌,制备成所需的聚酰胺酸溶液;其中改性纳米填料和增塑剂占聚酰胺酸溶液的质量比分别为2%和1%;所述改性纳米填料按重量份包括20-30份碳纤维、40-50份二氧化硅、10-15份四氟化硅以及5-10份碳化硅;
步骤二、制备可成型聚酰亚胺薄膜,将上述混合均匀的聚酰胺酸溶液经过真空脱泡后流延至钢带或者玻璃基材上,并在干燥惰性气体的保护下采用远红外加热的方式,具体是先在100-120℃保持10-20min,然后依次在140-160℃保持10-20min,在180-220℃保持10-20min,在220-280℃保持10-20min,在320-380℃保持10-20min,在380-400℃保持5-10min,经拉伸亚胺化得到聚酰亚胺薄膜。
2.根据权利要求1所述的可成型聚酰亚胺薄膜的制备方法,其特征在于:所述增塑剂为增塑剂选自邻苯二甲酸二辛脂(DOP)、邻苯二甲酸二丁脂(DBP)、过氧化二异丙苯(DCP)和邻苯二甲酸二乙脂(DEP)中的一种或几种。
3.根据权利要求1所述的可成型聚酰亚胺薄膜的制备方法,其特征在于:所述制备聚酰胺酸溶液中的二酐为均苯四甲酸二酐(PMDA)、氢化均苯四甲酸二酐(HPMDA)、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)中的两种或几种。
4.根据权利要求1所述的可成型聚酰亚胺薄膜的制备方法,其特征在于:所述二胺为4,4-二氨基二苯醚(4,4-ODA)、3,4’-二氨基二苯醚(3,4-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)、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)、1,3-二(4-氨基苯氧基)苯(1,3,4-APB)中的两种或几种。
5.根据权利要求1所述的可成型聚酰亚胺薄膜的制备方法,其特征在于:所述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。
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