CN107141476A - 一种薄型电子级聚酰亚胺薄膜的制备方法 - Google Patents
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Abstract
本发明公开了一种薄型电子级聚酰亚胺薄膜的制备方法,该方法的具体步骤如下:1)、将3,4′-BPDA和4-PEPA进行甲酯化,制得白色和淡黄色的酯化粉末(PDE和PEPE)。然后按照一定比例将BPDE、PEPE和二胺加入溶剂中,加热回流搅拌2h即得棕红色的合成聚酰胺酸液;2)、合成聚酰胺酸液经过滤、真空脱泡、流延成膜、双向拉伸、高温热定型处理、电晕处理、卷取工序,制得物理机械性能优良的电子级聚酰亚胺薄膜;3)、将经表面有机化改性的超细无机晶须和/或纳米粒子材料,借助高能量密度超声波的粉碎和空化作用,实现上述功能填料同本发明所述多元聚酰胺酸形成原位微纳复合可将聚酰亚胺薄膜亚胺化。
Description
技术领域
本发明涉及聚酰亚胺薄膜制备生产技术领域,具体为一种薄型电子级聚酰亚胺薄膜的制备方法。
背景技术
聚酰亚胺薄膜是一种新型的耐高温有机聚合物薄膜,是由均苯四甲酸二酐(PMDA)和二氨基二苯醚(ODA)在极强性溶剂二甲基乙酰胺(DMAC)中经缩聚并流涎成膜,再经亚胺化而成.它是目前世界上性能最好的薄膜类绝缘材料,具有优良的力学性能、电性能、化学稳定性以及很高的抗辐射性能、耐高温和耐低温性能(-269℃至+400℃)。
1959年美国杜邦公司首先合成出芳香族聚酰亚胺,1962年试制成聚酰亚胺薄膜(PI薄膜),1965年开始生产,商品牌号为KAPTON。
我国60年代末可以小批量生产聚酰亚胺薄膜,现在已广泛应用于航空、航海、宇宙飞船、火箭导弹、原子能、电子电器工业等各个领域。
目前,聚酰胺酸溶液存在不稳定对水汽很敏感,储存过程中常发生分解的问题。
发明内容
本发明的目的在于提供一种薄型电子级聚酰亚胺薄膜的制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种薄型电子级聚酰亚胺薄膜的制备方法,所述技术的步骤包括:
1)、将3,4′-BPDA和4-PEPA进行甲酯化,制得白色和淡黄色的酯化粉末(PDE和PEPE)。然后按照一定比例将BPDE、PEPE和二胺加入溶剂中,加热回流搅拌2h即得棕红色的合成聚酰胺酸液;
2)、合成聚酰胺酸液经过滤、真空脱泡、流延成膜、双向拉伸、高温热定型处理、电晕处理、卷取工序,制得物理机械性能优良的电子级聚酰亚胺薄膜;
3)、将经表面有机化改性的超细无机晶须和/或纳米粒子材料,借助高能量密度超声波的粉碎和空化作用,实现上述功能填料同本发明所述多元聚酰胺酸形成原位微纳复合可将聚酰亚胺薄膜亚胺化
4)、对步骤2)的流延成膜,消泡后的聚酰胺酸溶液,由不锈钢溶液储罐经管路压入前机头上的流涎嘴储槽中。钢带匀速运行,将储槽中的溶液经流涎嘴前刮板带走,而形成厚度均匀的液膜,然后进入烘干道干燥;
5)、对步骤2)复合胶液经过滤、真空脱泡,洁净干燥的空气由鼓风机送入加热器预热到一定温度后进入上、下烘干道,热风流动方向与钢带运行方向相反;
6)、对步骤3)中聚酰亚胺薄膜亚胺化,聚酰胺酸薄膜在钢带上随其运行一周,溶剂蒸发成为固态薄膜,从钢带上剥离下的薄膜经导向辊引向亚胺化炉。亚胺化炉一般为多辊筒形式,与流涎机同步速度的导向辊引导聚酰胺酸薄膜进入亚胺化炉,高温亚胺化后,由收卷机收卷。
优选的,所述步骤1)中,BPDE、PEPE和二胺在容剂中的计算固含量为40%(质量分数)。
优选的,所述步骤2)中,利电子级聚酰亚胺薄膜的制得厚度(7.5~125)μm、线胀系数5~18ppm/℃。
优选的,超细无机晶包括有氧化锌晶须、碳化硅晶须、钨酸锆晶须。
与现有技术相比,本发明的有益效果是:
该制备方法制造出的聚异酰亚胺结构稳定,作为聚酰亚胺的先母体,由于热处理时不会放出水等低分子物质,容易异构化成酰亚胺,能制得性能优良的聚酰亚胺。聚异酰亚胺是由聚酰胺酸在脱水剂作用下,脱水环化为聚异酰亚胺,然后在酸或碱等催化剂作用下异构化成聚酰亚胺,此异构化反应在高温下很容易进行;
聚异酰亚胺溶解性好,玻璃化转变温度较低,加工性能优良;
聚酰亚胺为不溶、不熔性材料,难于加工,通常采用先在预聚物聚酰亚胺阶段加工,但由于在高温下进行,亚胺化时闭环脱水易使制品产生气孔,导致制品的机械性能和电性能下降,难以获得理想的产品,作为聚酰亚胺预聚的聚异酰亚胺,其玻璃化温度低于对应的聚酰亚胺,热处理时不会放出水分,易异构化成聚酰亚胺,因此用聚异酰亚胺代替聚酰胺酸作为聚酰亚胺的前身材料,可制得性能优良的制品;
该法较新颖,正受到广泛关注。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明提供一种技术方案:一种薄型电子级聚酰亚胺薄膜的制备方法,包括以下步骤:
1)、将3,4′-BPDA和4-PEPA进行甲酯化,制得白色和淡黄色的酯化粉末(PDE和PEPE)。然后按照一定比例将BPDE、PEPE和二胺加入溶剂中,加热回流搅拌2h即得棕红色的合成聚酰胺酸液;
2)、合成聚酰胺酸液经过滤、真空脱泡、流延成膜、双向拉伸、高温热定型处理、电晕处理、卷取工序,制得物理机械性能优良的电子级聚酰亚胺薄膜;
3)、将经表面有机化改性的超细无机晶须和/或纳米粒子材料,借助高能量密度超声波的粉碎和空化作用,实现上述功能填料同本发明所述多元聚酰胺酸形成原位微纳复合可将聚酰亚胺薄膜亚胺化
4)、对步骤2)的流延成膜,消泡后的聚酰胺酸溶液,由不锈钢溶液储罐经管路压入前机头上的流涎嘴储槽中。钢带匀速运行,将储槽中的溶液经流涎嘴前刮板带走,而形成厚度均匀的液膜,然后进入烘干道干燥;
5)、对步骤2)复合胶液经过滤、真空脱泡,洁净干燥的空气由鼓风机送入加热器预热到一定温度后进入上、下烘干道。热风流动方向与钢带运行方向相反,以便使液膜在干燥时温度逐渐升高,溶剂逐渐挥发,增加干燥效果;
6)、对步骤3)中聚酰亚胺薄膜亚胺化,聚酰胺酸薄膜在钢带上随其运行一周,溶剂蒸发成为固态薄膜,从钢带上剥离下的薄膜经导向辊引向亚胺化炉。亚胺化炉一般为多辊筒形式,与流涎机同步速度的导向辊引导聚酰胺酸薄膜进入亚胺化炉,高温亚胺化后,由收卷机收卷。
进一步的,步骤2)中,利电子级聚酰亚胺薄膜的制得厚度(7.5~125)μm、线胀系数5~18ppm/℃。
进一步的,步骤3)中,超细无机晶包括有氧化锌晶须、碳化硅晶须、钨酸锆晶须。
尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (4)
1.一种薄型电子级聚酰亚胺薄膜的制备方法,其特征在于:包括以下步骤:
1)、将3,4′-BPDA和4-PEPA进行甲酯化,制得白色和淡黄色的酯化粉末(PDE和PEPE);然后按照一定比例将BPDE、PEPE和二胺加入溶剂中,加热回流搅拌2h即得棕红色的合成聚酰胺酸液;
2)、合成聚酰胺酸液经过滤、真空脱泡、流延成膜、双向拉伸、高温热定型处理、电晕处理、卷取工序,制得物理机械性能优良的电子级聚酰亚胺薄膜;
3)、将经表面有机化改性的超细无机晶须和/或纳米粒子材料,借助高能量密度超声波的粉碎和空化作用,实现上述功能填料同本发明所述多元聚酰胺酸形成原位微纳复合可将聚酰亚胺薄膜亚胺化;
4)、对步骤2)的流延成膜,消泡后的聚酰胺酸溶液,由不锈钢溶液储罐经管路压入前机头上的流涎嘴储槽中;钢带匀速运行,将储槽中的溶液经流涎嘴前刮板带走,而形成厚度均匀的液膜,然后进入烘干道干燥;
5)、对步骤2)复合胶液经过滤、真空脱泡,洁净干燥的空气由鼓风机送入加热器预热到一定温度后进入上、下烘干道;热风流动方向与钢带运行方向相反;
6)、对步骤3)中聚酰亚胺薄膜亚胺化,聚酰胺酸薄膜在钢带上随其运行一周,溶剂蒸发成为固态薄膜,从钢带上剥离下的薄膜经导向辊引向亚胺化炉;亚胺化炉一般为多辊筒形式,与流涎机同步速度的导向辊引导聚酰胺酸薄膜进入亚胺化炉,高温亚胺化后,由收卷机收卷。
2.根据权利要求1所述的一种薄型电子级聚酰亚胺薄膜的制备方法,其特征在于:所述步骤1)中,BPDE、PEPE和二胺在容剂中的计算固含量为40%(质量分数)。
3.根据权利要求1所述的一种薄型电子级聚酰亚胺薄膜的制备方法,其特征在于:所述步骤2)中,利电子级聚酰亚胺薄膜的制得厚度(7.5~125)μm、线胀系数5~18ppm/℃。
4.根据权利要求1所述的一种薄型电子级聚酰亚胺薄膜的制备方法,其特征在于:所述步骤3)中,超细无机晶包括有氧化锌晶须、碳化硅晶须、钨酸锆晶须。
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