CN113512214B - 一种阻隔性好的透明聚酰亚胺薄膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种阻隔性好的透明聚酰亚胺薄膜,所述阻隔性好的透明聚酰亚胺薄膜中掺杂有1.5‑2wt%氨基化氮化硼纳米片和7‑8wt%纳米二氧化硅。本发明还公开了上述阻隔性好的透明聚酰亚胺薄膜的制备方法,包括如下步骤:S1、在惰性气体氛围中,取氨基化氮化硼纳米片、二胺单体和二酐单体在有机溶液中反应得到聚酰胺酸溶液;然后加入含有氨基的硅烷偶联剂继续反应得到溶液A;S2、将溶液A与全氢聚硅氮烷溶液混匀,消泡得到溶液B;将溶液B涂覆于基板表面,亚胺化,冷却至室温,剥离得到阻隔性好的透明聚酰亚胺薄膜。本发明具有良好的阻隔性能。
Description
技术领域
本发明涉及聚酰亚胺技术领域,尤其涉及一种阻隔性好的透明聚酰亚胺薄膜及其制备方法。
背景技术
聚酰亚胺被称为“黄金塑料”,具有突出的热稳定性和尺寸稳定性,以及良好的分子结构可设计性等特点。聚酰亚胺被认为是柔性有机电致发光器件衬底材料的最佳选择之一。但是聚酰亚胺的阻隔水蒸气的性能相对较差,不能阻挡水对器件的阴极、有机发光等材料的侵蚀,限制了聚酰亚胺的应用。
发明内容
基于背景技术存在的技术问题,本发明提出了一种阻隔性好的透明聚酰亚胺薄膜及其制备方法,本发明具有良好的阻隔性能。
本发明提出了一种阻隔性好的透明聚酰亚胺薄膜,所述阻隔性好的透明聚酰亚胺薄膜中掺杂有1.5-2wt%氨基化氮化硼纳米片和7-8wt%纳米二氧化硅。
优选地,氨基化氮化硼纳米片为γ-氨丙基三乙氧基硅烷改性氮化硼纳米片。
本发明还提出了上述阻隔性好的透明聚酰亚胺薄膜的制备方法,包括如下步骤:
S1、在惰性气体氛围中,取氨基化氮化硼纳米片、二胺单体和二酐单体在有机溶液中反应得到聚酰胺酸溶液;然后加入含有氨基的硅烷偶联剂继续反应得到溶液A;
S2、将溶液A与全氢聚硅氮烷溶液混匀,消泡得到溶液B;将溶液B涂覆于基板表面,亚胺化,冷却至室温,剥离得到阻隔性好的透明聚酰亚胺薄膜。
上述二胺单体和二酐单体含有氟元素或酯环结构,可以获得透明的聚酰亚胺薄膜,如1,4-双(2'-三氟甲基-4'-氨基苯氧基)苯、4,4'-二氨基二环己基甲烷、4,4'-(六氟异丙烯)二酞酸酐、1,2,4,5-环己烷四羧酸二酐等。
上述含氨基的硅烷偶联剂可以为γ-氨丙基三乙氧基硅烷等。
优选地,在S1中,二胺单体、二酐单体、含氨基的硅烷偶联剂的摩尔比为0.92-0.94:1:0.04-0.06。
优选地,在S1中,于室温反应14-16h得到聚酰胺酸溶液;然后加入含有氨基的硅烷偶联剂继续反应1-2h得到溶液A。
优选地,在S1中,溶液A的固含量为15-18wt%。
优选地,在S1中,有机溶剂为N,N-二甲基乙酰胺、N,N-二甲基甲酰胺中的至少一种。
优选地,在S2中,全氢聚硅氮烷溶液的溶剂为N,N-二甲基乙酰胺、N,N-二甲基甲酰胺中的至少一种。
优选地,在S2中,亚胺化程序为:分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温0.5-1.5h。
有益效果:
本发明选用氨基化氮化硼纳米片、二胺单体和二酐单体进行反应,使得聚酰胺酸中接枝氨基化氮化硼纳米片均匀分散并接枝在聚酰胺酸中,可以提高本发明的阻隔水蒸气的性能;
聚酰胺酸溶液与含氨基的硅烷偶联剂反应,接枝上偶联剂;再与全氢聚硅氮烷溶液均匀分散,全氢聚硅氮烷容易水解成均匀分散的纳米二氧化硅,并通过硅烷偶联剂使得纳米二氧化硅与聚酰胺酸连接在一起,并包覆纳米二氧化硅,纳米二氧化硅与氮化硼纳米片相互配合可以大幅提高薄膜阻隔水蒸气的性能;另外均匀分布的纳米二氧化硅和氮化硼纳米片,在提高薄膜阻隔性能的同时保持良好的透明性能。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种阻隔性好的透明聚酰亚胺薄膜,所述阻隔性好的透明聚酰亚胺薄膜中掺杂有1.5wt%γ-氨丙基三乙氧基硅烷改性氮化硼纳米片和8wt%纳米二氧化硅。
上述阻隔性好的透明聚酰亚胺薄膜的制备方法,包括如下步骤:
S1、将1.05gγ-氨丙基三乙氧基硅烷改性氮化硼纳米片与400mlN,N-二甲基乙酰胺混匀,超声分散20min,然后加入0.092mol 4,4’-二氨基二环己基甲烷混匀溶解,通入氮气,然后分5次加入4,4'-(六氟异丙烯)二酞酸酐(共0.1mol)混匀,于室温反应14h得到聚酰胺酸溶液;然后加入0.006molγ-氨丙基三乙氧基硅烷继续反应2h得到溶液A;
S2、将溶液A与质量分数为10wt%全氢聚硅氮烷的N,N-二甲基乙酰胺42ml混匀,消泡得到溶液B;将溶液B涂覆于基板表面,在氮气氛围中,分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温0.5h,冷却至室温,剥离得到阻隔性好的透明聚酰亚胺薄膜。
实施例2
一种阻隔性好的透明聚酰亚胺薄膜,所述阻隔性好的透明聚酰亚胺薄膜中掺杂有2wt%γ-氨丙基三乙氧基硅烷改性氮化硼纳米片和7wt%纳米二氧化硅。
上述阻隔性好的透明聚酰亚胺薄膜的制备方法,包括如下步骤:
S1、将1.4gγ-氨丙基三乙氧基硅烷改性氮化硼纳米片与400mlN,N-二甲基乙酰胺混匀,超声分散20min,然后加入0.094mol 4,4’-二氨基二环己基甲烷混匀溶解,通入氮气,然后分5次加入4,4'-(六氟异丙烯)二酞酸酐(共0.1mol)混匀,于室温反应16h得到聚酰胺酸溶液;然后加入0.004molγ-氨丙基三乙氧基硅烷继续反应1h得到溶液A;
S2、将溶液A与质量分数为10wt%全氢聚硅氮烷的N,N-二甲基乙酰胺37ml混匀,消泡得到溶液B;将溶液B涂覆于基板表面,在氮气氛围中,分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温1.5h,冷却至室温,剥离得到阻隔性好的透明聚酰亚胺薄膜。
实施例3
一种阻隔性好的透明聚酰亚胺薄膜,所述阻隔性好的透明聚酰亚胺薄膜中掺杂有1.7wt%γ-氨丙基三乙氧基硅烷改性氮化硼纳米片和7.5wt%纳米二氧化硅。
上述阻隔性好的透明聚酰亚胺薄膜的制备方法,包括如下步骤:
S1、将1.2gγ-氨丙基三乙氧基硅烷改性氮化硼纳米片与400mlN,N-二甲基乙酰胺混匀,超声分散20min,然后加入0.093mol 4,4’-二氨基二环己基甲烷混匀溶解,通入氮气,然后分5次加入4,4'-(六氟异丙烯)二酞酸酐(共0.1mol)混匀,于室温反应15h得到聚酰胺酸溶液;然后加入0.005molγ-氨丙基三乙氧基硅烷继续反应1.5h得到溶液A;
S2、将溶液A与质量分数为10wt%全氢聚硅氮烷的N,N-二甲基乙酰胺39ml混匀,消泡得到溶液B;将溶液B涂覆于基板表面,在氮气氛围中,分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温1h,冷却至室温,剥离得到阻隔性好的透明聚酰亚胺薄膜。
对比例1
一种透明聚酰亚胺薄膜的制备方法,包括如下步骤:
将0.093mol 4,4’-二氨基二环己基甲烷与400mlN,N-二甲基乙酰胺混匀溶解,通入氮气,然后分5次加入4,4'-(六氟异丙烯)二酞酸酐(共0.1mol)混匀,于室温反应15h得到聚酰胺酸溶液;消泡后将聚酰胺酸溶液涂覆于基板表面,在氮气氛围中,分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温1h,冷却至室温,剥离得到透明聚酰亚胺薄膜。
对比例2
一种透明聚酰亚胺薄膜的制备方法,包括如下步骤:
将1.2gγ-氨丙基三乙氧基硅烷改性氮化硼纳米片与400mlN,N-二甲基乙酰胺混匀,超声分散20min,然后加入0.093mol 4,4’-二氨基二环己基甲烷混匀溶解,通入氮气,然后分5次加入4,4'-(六氟异丙烯)二酞酸酐(共0.1mol)混匀,于室温反应15h得到聚酰胺酸溶液;
将聚酰胺酸溶液涂覆于基板表面,在氮气氛围中,分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温1h,冷却至室温,剥离得到透明聚酰亚胺薄膜。
对比例3
一种透明聚酰亚胺薄膜的制备方法,包括如下步骤:
将0.093mol 4,4’-二氨基二环己基甲烷与400mlN,N-二甲基乙酰胺混匀溶解,通入氮气,然后分5次加入4,4'-(六氟异丙烯)二酞酸酐(共0.1mol)混匀,于室温反应15h得到聚酰胺酸溶液;
S2、将聚酰胺酸溶液与质量分数为10wt%全氢聚硅氮烷的N,N-二甲基乙酰胺39ml混匀,消泡;然后涂覆于基板表面,在氮气氛围中,分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温1h,冷却至室温,剥离得到透明聚酰亚胺薄膜。
取实施例1-3和对比例1-3制得的薄膜,进行性能检测,结果如表1所示。
参照ASTMF-1249,检测薄膜的水蒸气透过率,测试面积为5cm2,相对湿度为90%。
表1检测结果
由上表可以看出,本发明具有良好的阻隔性能和透明性。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (9)
1.一种阻隔性好的透明聚酰亚胺薄膜,其特征在于,所述阻隔性好的透明聚酰亚胺薄膜中掺杂有1.5-2wt%氨基化氮化硼纳米片和7-8wt%纳米二氧化硅;
所述阻隔性好的透明聚酰亚胺薄膜的制备方法,包括如下步骤:
S1、在惰性气体氛围中,取氨基化氮化硼纳米片、二胺单体和二酐单体在有机溶液中反应得到聚酰胺酸溶液;然后加入含有氨基的硅烷偶联剂继续反应得到溶液A;
S2、将溶液A与全氢聚硅氮烷溶液混匀,消泡得到溶液B;将溶液B涂覆于基板表面,亚胺化,冷却至室温,剥离得到阻隔性好的透明聚酰亚胺薄膜。
2.根据权利要求1所述阻隔性好的透明聚酰亚胺薄膜,其特征在于,氨基化氮化硼纳米片为γ-氨丙基三乙氧基硅烷改性氮化硼纳米片。
3.一种如权利要求1或2所述阻隔性好的透明聚酰亚胺薄膜的制备方法,其特征在于,包括如下步骤:
S1、在惰性气体氛围中,取氨基化氮化硼纳米片、二胺单体和二酐单体在有机溶液中反应得到聚酰胺酸溶液;然后加入含有氨基的硅烷偶联剂继续反应得到溶液A;
S2、将溶液A与全氢聚硅氮烷溶液混匀,消泡得到溶液B;将溶液B涂覆于基板表面,亚胺化,冷却至室温,剥离得到阻隔性好的透明聚酰亚胺薄膜。
4.根据权利要求3所述阻隔性好的透明聚酰亚胺薄膜的制备方法,其特征在于,在S1中,二胺单体、二酐单体、含氨基的硅烷偶联剂的摩尔比为0.92-0.94:1:0.04-0.06。
5.根据权利要求3或4所述阻隔性好的透明聚酰亚胺薄膜的制备方法,其特征在于,在S1中,于室温反应14-16h得到聚酰胺酸溶液;然后加入含有氨基的硅烷偶联剂继续反应1-2h得到溶液A。
6.根据权利要求3或4所述阻隔性好的透明聚酰亚胺薄膜的制备方法,其特征在于,在S1中,溶液A的固含量为15-18wt%。
7.根据权利要求3或4所述阻隔性好的透明聚酰亚胺薄膜的制备方法,其特征在于,在S1中,有机溶剂为N,N-二甲基乙酰胺、N,N-二甲基甲酰胺中的至少一种。
8.根据权利要求3或4所述阻隔性好的透明聚酰亚胺薄膜的制备方法,其特征在于,在S2中,全氢聚硅氮烷溶液的溶剂为N,N-二甲基乙酰胺、N,N-二甲基甲酰胺中的至少一种。
9.根据权利要求3或4所述阻隔性好的透明聚酰亚胺薄膜的制备方法,其特征在于,在S2中,亚胺化程序为:分别于70-80℃、110-120℃、150-170℃、220-240℃和330-350℃保温0.5-1.5h。
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