CN111647182A - 一种高固含量的无色透明聚酰亚胺薄膜制备方法 - Google Patents
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Abstract
本申请公开了一种高固含量的无色透明聚酰亚胺薄膜制备方法。本申请的无色透明聚酰亚胺是由多组分含氟及脂肪环结构的二酸酐或二胺结构通过加热聚合成聚酰胺酸胶体、涂布成膜和分段加热的方式生成的无色透明聚酰亚胺薄膜。与正常方法制备的透明聚酰亚胺相比，具备较高的无色透光性和拉伸强度以及良好的阻水阻氧效果。此材料可应用于折叠屏幕制备过程中的透明基底以及柔性太阳能电池板基底，能够长期在耐受高温条件下工作并仍旧保持较高的无色透明度和可弯折回弹恢复性能。
Description
技术领域
本申请设计聚合物材料领域，特别是涉及一种高固含量的无色透明聚酰亚胺薄膜制备方法。
背景技术
聚酰亚胺是指主链上含有酰胺基团(-CO-NH-CO-)的高分子聚合物。由于其在耐高低温方面性能极佳，可在-200℃到+400℃间保持不变形，且具有一定的防辐射性能。被广泛的应用于航空、航天和微电子等技术领域。当今对性能优异的聚酰亚胺材料来说，降低其黄色外观，提高其光学性能是目前聚酰亚胺行业面临的一大难题。无色透明聚酰亚胺是由多组分含氟及脂肪环结构的二酸酐或二胺结构通过加热聚合成聚酰胺酸胶体、涂布成膜和分段加热的方式生成的无色透明聚酰亚胺薄膜。正常方法制备的透明聚酰亚胺相比，具备较高的无色透光性和拉伸强度以及良好的阻水阻氧效果。此材料可应用于折叠屏幕制备过程中的透明基底以及柔性太阳能电池板基底，能够长期在耐受高温条件下工作并仍旧保持较高的无色透明度和可弯折回弹恢复性能。
发明内容
本发明的目的是提供一种高固含量的无色透明聚酰亚胺薄膜制备方法，该方法制成的聚酰亚胺具有在其他方面性能不变甚至更优的情况下，其黄色外观变成无色透明。有利于在透明基底以及柔性太阳能电池板基底的应用。
一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：其聚合物重复结构单元应为：
如图1所示
其中包含重复单元结构X1的二酸酐反应单体应为以下单体中的一种或多种：
如图2所示
其中包含重复单元结构X2的二胺反应单体应为以下单体中的一种或多种：
如图3所示
其特征在于：所述的无色透明聚酰胺酸胶体制备方法包括：
a1、将含有X1结构的二酸酐与和X2结构的二胺的按照摩尔比为 (0.98～1.10)称重；
a2、在惰性气氛中先将含有X2结构的二胺迅速溶在极性非质子有机溶剂的烧杯中，控温在0～55℃的条件下200～400r/min持续搅拌，待均匀溶解后，再在5～15min内将含有X1结构的二酸酐单体逐步加入完成并继续在 80～120℃中以300～400r/min持续搅拌后得到无色透明的均相、粘稠的聚酰胺酸胶体；
a3、将所得无色透明聚酰胺酸溶液涂布到光洁的玻璃板上，在烘箱中先后经历低中高三个温度段各自5～25min；
a4、最终取出玻璃板待完全冷却后揭起薄膜即可得到无色的聚酰亚胺薄膜。
其特征在于：步骤a2中最终总体含有结构的二酸酐与二胺的总质量占反应物料总质量的10～40％。
其特征在于：步骤a2的惰性气体分别为氮气、氩气、氦气中的一种或多种。
其特征在于：步骤a2中的连续搅拌时间为12～72h。
其特征在于：步骤a2所述的极性溶剂为N-甲基吡咯烷酮(NMP)、 N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)、四氢呋喃(THF)、二甲基矾(MSM)、二甲基亚矾(DMSO)。
其特征在于：步骤a3低温度段为60～100℃；中温度段为230～280℃；高温度段为330～400℃。
附图说明
图1为聚合物重复结构单元示意图；
图2为重复单元结构X1的二酸酐反应单体示意图；
图3为重复单元结构X2的二胺反应单体示意图。
具体实施方式
聚酰亚胺作为一大类高分子聚合物，制备聚酰亚胺的单体有两百种以上，由于选用的单体不同，所制备的聚酰亚胺存在着性能差异。本申请通过大量的研究，发现带有含氟基团和脂肪族基团的单体制备的聚酰亚胺具备较好的无色透光性和拉伸强度以及良好的阻水阻氧效果。且在耐辐射、耐高低温方面具有良好的性能。
下面通过具体的实施例对本申请作进一步详细说明，以下实施例仅对本申请进行进一步说明，不应理解为对本申请的限制。
实施例1:
室温下在氮气气氛中将1.8424g(联苯胺)加入50ml烧杯内，溶解在10.4643g 的30℃和250r/min搅拌速率的极性非质子溶剂DMAc中，充分溶解后在10分钟内缓慢加入2.6423g(5-(2,5-二氧四氢呋喃)-3-甲基-3-环己烯-1,2-二碳酸酐)，随后升温至120℃以350r/min的速率持续搅拌48h，最终得到无色透明的聚酰胺酸胶体；然后将所得无色透明胶体倾倒在光洁玻璃板上涂布，随后在烘箱中经历30min的80℃、10min的250℃、15min 的350℃；待完全冷却后揭起即可得无色透明的聚酰亚胺薄膜。
实施例2：
室温下在氩气气气氛中将4.3249g(双[4-(4-氨基苯氧基)苯基]砜)加入三口烧瓶内，溶解在16.2568g的40℃和300r/min搅拌速率的极性非质子溶剂DMAc中，充分溶解后在8分钟内缓慢加入2.6423g(5-(2,5-二氧四氢呋喃)-3-甲基-3-环己烯-1,2-二碳酸酑)，随后持续搅拌12h获得均相蓝色的粘稠聚酰胺酸胶体；取出胶体倾倒在光洁玻璃板上，分别经历10min的90℃、15min的260℃、15min的360℃；待完全冷却后揭起即可得蓝色的聚酰亚胺薄膜。
实施例3：
室温下在氩气气气氛中将1.0012g(4,4'-二氨基二苯醚)和0.9212g(联苯胺)加入三口烧瓶内，溶解在12.84547g的40℃和300r/min搅拌速率的极性非质子溶剂DMAc 中，充分溶解后在8分钟内缓慢加入3.5828g(3,3,4,4-二苯基砜四羧酸二酸酐)，随后持续搅拌12h获得均相蓝色的粘稠聚酰胺酸胶体；取出胶体倾倒在光洁玻璃板上，分别经历 10min的90℃、15min的260℃、15min的360℃；待完全冷却后揭起即可得蓝色的聚酰亚胺薄膜。
经过使用本发明所提供的透明聚酰亚胺制备方法所得薄膜，热稳定性、拉伸强度、耐折叠性、阻水阻氧效果都与正常的聚酰亚胺薄膜性能相当。
以上内容是结合具体的实施方式对本申请所作的进一步详细说明，不能认定本申请的具体实施只限于这些说明。对于本申请所属技术领域的技术人员来说，在不脱离本申请的构思的前提下，还可做出简单的替换，都应当视为属于本申请的保护范围。
Claims (7)
1.一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：其聚合物重复结构单元应为：
其中：X1、X2选自以下结构通式中的一种或多种，其中包含重复单元结构X1的二酸酐反应单体应为以下单体中的一种或多种：
其中包含重复单元结构X2的二胺反应单体应为以下单体中的一种或多种：
2.根据权利要求1所述一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：所述的无色透明聚酰胺酸胶体制备方法包括：
a1、将含有X1结构的二酸酐与和X2结构的二胺的按照摩尔比为(0.98～1.10)称重；
a2、在惰性气氛中先将含有X2结构的二胺迅速溶在极性非质子有机溶剂的烧杯中，控温在0～55℃的条件下200～400r/min持续搅拌，待均匀溶解后，再在5～15min内将含有X1结构的二酸酐单体逐步加入完成并继续在80～120℃中以300～400r/min持续搅拌后得到无色透明的均相、粘稠的聚酰胺酸胶体；
a3、将所得无色透明聚酰胺酸溶液涂布到光洁的玻璃板上，在烘箱中先后经历低中高三个温度段各自5～25min；
a4、最终取出玻璃板待完全冷却后揭起薄膜即可得到无色的聚酰亚胺薄膜。
3.根据权利要求2所述一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：步骤a2中最终总体含有结构的二酸酐与二胺的总质量占反应物料总质量的10～40％。
4.根据权利要求2所述一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：步骤a2的惰性气体分别为氮气、氩气、氦气中的一种或多种。
5.根据权利要求2所述一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：步骤a2中的连续搅拌时间为12～72h。
6.根据权利要求2所述一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：步骤a2所述的极性溶剂为N-甲基吡咯烷酮(NMP)、N，N-二甲基甲酰胺(DMF)、N，N-二甲基乙酰胺(DMAc)、四氢呋喃(THF)、二甲基矾(MSM)、二甲基亚矾(DMSO)。
7.根据权利要求2所述一种高固含量的无色透明聚酰亚胺薄膜制备方法，其特征在于：步骤a3低温度段为60～100℃；中温度段为230～280℃；高温度段为330～400℃。
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