CN111808526A - 一种uv固化聚苯胺/聚氨酯导电涂层的制备方法 - Google Patents

一种uv固化聚苯胺/聚氨酯导电涂层的制备方法 Download PDF

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CN111808526A
CN111808526A CN202010747881.9A CN202010747881A CN111808526A CN 111808526 A CN111808526 A CN 111808526A CN 202010747881 A CN202010747881 A CN 202010747881A CN 111808526 A CN111808526 A CN 111808526A
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姚伯龙
王宇通
陈欢
王海潮
倪亚洲
程广鸿
张晋瑞
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Jiangnan University
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Abstract

一种UV固化聚苯胺/聚氨酯导电涂层的制备方法，属于水性聚氨酯制备技术领域。本发明以水性聚氨酯为基体材料，在该体系中加入多羟基丙烯酸酯，多羟基丙烯酸酯不单是UV固化单体，而且还在合成水性聚氨酯的过程中起到了稀释剂的作用，减少了体系中的溶剂含量。在固化成膜的过程中，分子发生交联反应，膜表面的结构会变得更加紧密。在合成了水性聚氨酯乳液的基础上，继续与导电填料聚苯胺进行共混，可以使得到的涂层在保证机械强度的同时，满足耐热性、耐水性等性能要求，并具有较好的导电性和抗静电性。

Description

一种UV固化聚苯胺/聚氨酯导电涂层的制备方法
技术领域
本发明涉及一种UV固化聚苯胺/聚氨酯导电涂层的制备方法，属于水性聚氨酯制备技术领域。
背景技术
八十年代以来，导电聚合物逐渐成为了导电涂料中重要的导电填料。聚苯胺就是发现较早并经过系统研究的导电聚合物之一。聚苯胺因其具有的原料易得、合成工艺简单、化学及环境稳定性好等特点而得到了广泛的研究和应用。目前，聚苯胺成为了研究最广的导电聚合物之一。
水性聚氨酯以水为溶剂，具有无污染、安全可靠、机械性能优良、相容性好、易于改性等优点。
由于UV固化技术固化速度快、固化时间短、固化温度低、绿色环保以及聚氨酯材料成膜性能较好，因此以UV固化聚氨酯为成膜树脂，将其与导电高聚物填料聚苯胺复合，制备UV固化导电涂料，使得我们制备的涂层在机械强度、热性能、耐水性等性能满足要求的前提下，同时具备较好的导电性和抗静电性。
发明内容
本发明的目的是克服上述不足之处，提供一种UV固化聚苯胺/聚氨酯导电涂层的制备方法，其绿色环保、可导电，采用UV固化制备得到的水性聚氨酯。
本发明的技术方案，一种UV固化聚苯胺/聚氨酯导电涂层的制备方法，步骤如下：
（1）PU预聚物的合成：将装有聚四亚甲基醚二醇PTMG和1,4-丁二醇BDO的烧瓶放在60-80℃干燥烘箱中干燥1-2h；将二异氰酸酯和催化剂添加到烧瓶中，随后将烧瓶放在油浴锅中，60-80℃、300-400 r/min搅拌反应1.5-2.5h；
（2）WPU预聚物的合成：将溶解在溶剂A中的扩链剂倒入步骤（1）所得反应液中，反应1-2h，得到WPU预聚物；
（3）UV-WPU乳液的合成：当步骤（2）中的反应液温度降至35-45℃时，将得到的WPU预聚物和活性封端剂倒入步骤（1）制备所得的PU预聚物中，反应1-2h后，将双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯DPHA / DPGDA单体倒入PU预聚物中，反应1-2h后，将中和剂和去离子水加入烧瓶中，并将搅拌器的旋转速度增加至800-1000r/min，连续搅拌0.5-1h，得到UV-WPU乳液；
（4）PANI/WPU乳液的合成：在合成UV-WPU的基础上，使其与导电聚苯胺PANI进行共混1-2h，制备得到聚苯胺/聚氨酯PANI/WPU乳液；对其进行UV照射后固化成膜，得到聚苯胺/聚氨酯导电涂层。
进一步地，步骤（1）中聚四亚甲基醚二醇PTMG的量为0.005-0.015mol，1,4-丁二醇BDO的量为0.015-0.05mol；二异氰酸酯的加入量为0.04-0.06mol，催化剂的加入量为0.01-0.03g。
进一步地，步骤（1）中所述催化剂为二月桂酸二丁基锡和/或辛酸亚锡；
所述二异氰酸酯具体为甲苯二异氰酸酯TDI、4,4'-二苯基甲烷二异氰酸酯MDI及异佛尔酮二异氰酸酯IPDI中的一种或几种。
进一步地，步骤（2）中所述扩链剂在溶剂A中的浓度为7-10mol/L；扩链剂的加入量为0.01-0.012mol。
进一步地，步骤（2）中所述扩链剂具体为二羟甲基丙酸DMPA和/或二羟甲基丁酸DMBA；所述溶剂A具体为丙酮、丁酮及N,N-二甲基甲酰胺中的一种或几种。
进一步地，步骤（3）中活性封端剂的加入量为0.01-0.012mol；加入的双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯DPHA / DPGDA占PU预聚体重量的40 %；
加入中和剂进行中和，加入的量为0.01-0.012mol，充分反应后取出部分样品，滴加1-2滴酚酞试剂判断pH；随后加入50-80g去离子水。
进一步地，所述双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯DPHA / DPGDA的比例为1：1。
进一步地，步骤（3）中所述活性封端剂为丙烯酸羟乙酯HEA、甲基丙烯酸羟乙酯HEMA及季戊四醇三丙烯酸酯PETA中的一种或几种；所述中和剂为三乙胺。
进一步地，步骤（4）中加入的导电聚苯胺PANI占UV-WPU乳液质量的10%；共混后用紫外光（波长385nm）进行固化45-70s后成膜。
本发明以水性聚氨酯为基体材料，在该体系中加入多羟基丙烯酸酯，多羟基丙烯酸酯不单是UV固化单体，而且还在合成水性聚氨酯的过程中起到了稀释剂的作用，减少了体系中的溶剂含量。在固化成膜的过程中，分子发生交联反应，膜表面的结构会变得更加紧密。在合成了水性聚氨酯乳液的基础上，继续与导电填料聚苯胺进行共混，可以使得到的涂层在保证机械强度、耐热性、耐水性等性能满足要求的前提下，同时具有较好的导电性和抗静电性。
本发明的有益效果：本发明制备得到的涂层在保证机械强度，耐热性、耐水性等性能满足要求的前提下，同时具有较好的导电性和抗静电性，可广泛应用于移动通信系统天线、电台、电视台、输电网络或线路等。
附图说明
图1是实施例1制备所得的UV固化PANI/WPU膜的电导率半衰期曲线图。
图2是实施例1制备所得的UV固化PANI/WPU膜的静电半衰期曲线图。
具体实施方式
实施例1
（1）PU预聚物的合成：将装有2.5g ﹙0.01mol﹚聚四亚甲基醚二醇（PTMG）和0.9 g﹙0.01mol﹚ 1,4-丁二醇（BDO）的烧瓶放在 80 ℃的真空干燥烘箱中干燥 2 h，以除去药品中的水分。将8.89g﹙0.04mol﹚的异佛尔酮二异氰酸酯（IPDI）和0.03g﹙4.75x10-5mol﹚二月桂酸二丁基锡（DBTDL）添加到烧瓶中；随后将烧瓶放在油浴锅中，实验温度控制在70 ℃，机械搅拌器的转速控制在 360 r/min，实验反应时间为2 h。
（2）WPU预聚物的合成：将溶解在3.5g﹙0.048mol﹚ N，N-二甲基甲酰胺（DMF）中的1.35g﹙0.01mol﹚二羟甲基丙酸（DMPA）倒入烧瓶中。反应进行1 h，得到WPU预聚物。
（3）UV-WPU乳液的合成：当得到的WPU预聚物温度降至40℃时，将3.1g﹙0.01mol﹚季戊四醇三丙烯酸酯（PETA）倒入PU预聚物中，反应1 h后，将双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯（DPHA / DPGDA）单体倒入PU预聚物中，其中双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯（DPHA / DPGDA） 占 PU 预聚体的40 wt%。1 h后，将1.2g﹙0.012mol﹚三乙胺（TEA）和去离子水加入烧瓶中，使pH为中性，并将搅拌器的旋转速度增加至800 r/min，连续搅拌0.5 h，得到UV-WPU乳液。
（4）PANI/WPU乳液的合成:在合成UV-WPU的基础上，使其与适量导电聚苯胺（PANI）进行共混，制备了聚苯胺/聚氨酯（PANI/WPU）乳液，经UV照射后可固化成膜。
应用实施例1
采用实施例1所述制备方法，分别加入不同含量的导电聚苯胺（PANI），随后对制备所得的PANI/WPU膜进行电导率测试，采用四探针测试仪测量出来的是样品的电阻，待测样品为长方体，其尺寸为40 mm×10 mm×0.1 mm，在室温为23 ℃，相对湿度≤70%的条件下对样品进行测量，每组样品测量五次，取平均值，计算电导率。
具体结果如图1所示，可以发现，随着PANI含量的增加，PANI/WPU膜的电导率也逐渐增加，并且在PANI含量从5 wt%~10wt%时，PANI/WPU膜的导电率有一个大幅度的增长，之后电导率的增加十分缓慢，根据渗滤理论可以发现PANI的渗滤阈值是 10 wt%，当导电填料PANI 含量为10 wt%时，涂膜的电导率为 3.56×10-3 S/cm，符合导电的要求。
应用实施例2
采用实施例1所述制备方法，分别加入不同含量的导电聚苯胺（PANI）（具体含量），随后对制备所得的PANI/WPU膜进行静电半衰期测试,采用 LFY-401C 型静电半衰期测试仪对样品的静电半衰期进行测量。静电电压值的测量范围为 0~10 Kv，样品尺寸为 60 mm×80mm，每组样品测试三次，测量结果取平均值。
具体结果如图2所示，随着 PANI 含量的增加，PANI/WPU膜的静电半衰期逐渐减小，并在PANI含量5 wt%~10wt%之间时，有一个较大幅度的下降，这主要是因为PANI/WPU膜中有大量的PANI粒子，形成了足够多的导电通道，极大地改善了膜的抗静电性，之后静电半衰期的下降十分缓慢。当 PANI 含量为10 wt%时，PANI/WPU膜的静电半衰期为1.92 s，符合抗静电的要求。

Claims (9)

1.一种UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于步骤如下：
（1）PU预聚物的合成：将装有聚四亚甲基醚二醇PTMG和1,4-丁二醇BDO的烧瓶放在60-80℃干燥烘箱中干燥1-2h；将二异氰酸酯和催化剂添加到烧瓶中，随后将烧瓶放在油浴锅中，60-80℃、300-400 r/min搅拌反应1.5-2.5h；
（2）WPU预聚物的合成：将溶解在溶剂A中的扩链剂倒入步骤（1）所得反应液中，反应1-2h，得到WPU预聚物；
（3）UV-WPU乳液的合成：当步骤（2）中的反应液温度降至35-45℃时，将得到的WPU预聚物和活性封端剂倒入步骤（1）制备所得的PU预聚物中，反应1-2h后，将双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯DPHA / DPGDA单体倒入PU预聚物中，反应1-2h后，将中和剂和去离子水加入烧瓶中，并将搅拌器的旋转速度增加至800-1000r/min，连续搅拌0.5-1h，得到UV-WPU乳液；
（4）PANI/WPU乳液的合成：在合成UV-WPU的基础上，使其与导电聚苯胺PANI进行共混1-2h，制备得到聚苯胺/聚氨酯PANI/WPU乳液；对其进行UV照射后固化成膜，得到聚苯胺/聚氨酯导电涂层。
2.根据权利要求1所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：步骤（1）中聚四亚甲基醚二醇PTMG的量为0.005-0.015mol，1,4-丁二醇BDO的量为0.015-0.05mol；二异氰酸酯的加入量为0.04-0.06mol，催化剂的加入量为0.01-0.03g。
3.根据权利要求1所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：步骤（1）中所述催化剂为二月桂酸二丁基锡和/或辛酸亚锡；
所述二异氰酸酯具体为甲苯二异氰酸酯TDI、4,4'-二苯基甲烷二异氰酸酯MDI及异佛尔酮二异氰酸酯IPDI中的一种或几种。
4.根据权利要求1所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：步骤（2）中所述扩链剂在溶剂A中的浓度为7-10mol/L；扩链剂的加入量为0.01-0.012mol。
5.根据权利要求1所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：步骤（2）中所述扩链剂具体为二羟甲基丙酸DMPA和/或二羟甲基丁酸DMBA；所述溶剂A具体为丙酮、丁酮及N,N-二甲基甲酰胺中的一种或几种。
6.根据权利要求1所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：步骤（3）中活性封端剂的加入量为0.01-0.012mol；加入的双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯DPHA / DPGDA占PU预聚体重量的40 %；
加入中和剂进行中和，加入的量为0.01-0.012mol，充分反应后取出部分样品，滴加1-2滴酚酞试剂判断pH中性；随后加入50-80g去离子水。
7.根据权利要求6所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：所述双季戊四醇六丙烯酸酯/二丙二醇二丙烯酸酯DPHA / DPGDA的比例为1：1。
8.根据权利要求1所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：步骤（3）中所述活性封端剂为丙烯酸羟乙酯HEA、甲基丙烯酸羟乙酯HEMA及季戊四醇三丙烯酸酯PETA中的一种或几种；所述中和剂为三乙胺。
9.根据权利要求1所述UV固化聚苯胺/聚氨酯导电涂层的制备方法，其特征在于：步骤（4）中加入的导电聚苯胺PANI占UV-WPU乳液质量的10%；共混后用波长385nm紫外光进行固化45-70s后成膜。
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