CN108485261A - 一种聚苯胺导电薄膜 - Google Patents

一种聚苯胺导电薄膜 Download PDF

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CN108485261A
CN108485261A CN201810408330.2A CN201810408330A CN108485261A CN 108485261 A CN108485261 A CN 108485261A CN 201810408330 A CN201810408330 A CN 201810408330A CN 108485261 A CN108485261 A CN 108485261A
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顾黎明
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Abstract

本发明公开了一种聚苯胺导电薄膜,它是由下述重量份的原料制成的:硬脂酸3‑4份、苯胺120‑140份、引发剂3‑5份、十二烷基硫醇1‑2份、掺杂剂1‑2份、三丁基三氯化锡0.3‑0.5份、溶剂170‑200份、叔丁基对二苯酚0.8‑1份、轻质碳酸钙6‑8份、聚四氟乙烯蜡2‑3份、硅烷偶联剂kh560 0.7‑1份。本发明在苯胺聚合过程中引入了酸掺杂剂,能够有效地提高聚苯胺成品的导电稳定性,同时加入的叔丁基对二苯酚则能够提高聚苯胺导电薄膜的贮存稳定性。

Description

一种聚苯胺导电薄膜
技术领域
本发明属于薄膜领域,具体涉及一种聚苯胺导电薄膜。
背景技术
在目前已发现的导电高分子中,聚苯胺因其合成简单、价格低廉、电导率可调、环境稳定性好等诸多优点,尤其它在金属腐蚀防护、静电释放、电磁干扰屏蔽等领域有大规模应用的前景,成为研究最为广泛的一类导电高分子材料;然而为了更进一步的提高聚苯胺的导电性能,增大其应用领域,目前往往会将其与导电无机粒子共混,这样虽然可以提高导电性能,但是由于无机粒子与聚苯胺的相容性差,也会造成成品的稳定性差,尤其是做成复合薄膜时,更容易造成薄膜的均匀稳定性不好,导电薄膜的品质降低。
发明内容
本发明的目的在于针对现有技术的缺陷和不足,提供一种聚苯胺导电薄膜。
为实现上述目的,本发明采用以下技术方案:
一种聚苯胺导电薄膜,它是由下述重量份的原料制成的:
硬脂酸3-4份、苯胺120-140份、引发剂3-5份、十二烷基硫醇1-2份、掺杂剂1-2份、三丁基三氯化锡0.3-0.5份、溶剂170-200份、叔丁基对二苯酚0.8-1份、轻质碳酸钙6-8份、聚四氟乙烯蜡2-3份、硅烷偶联剂kh560 0.7-1份。
所述的掺杂剂选自对甲基苯磺酸或柠檬酸中的一种。
所述的引发剂选自过硫酸铵、过硫酸钾或过硫酸钠中的一种。
所述的溶剂为体积比为1:5-7的丙酮与二甲基甲酰胺的混合溶液。
优选地,本发明所述的聚苯胺导电薄膜,由包括以下步骤制得:
(1)取引发剂,加入到其重量25-30倍的去离子水中,搅拌均匀,得引发剂水溶液;
(2)取硅烷偶联剂kh560,加入到其重量10-13倍的无水乙醇中,升高温度为55-60℃,加入十二烷基硫醇,保温搅拌4-20分钟,得复合硅烷溶液;
(3)取硬脂酸,加热熔化,与轻质碳酸钙混合,加入到混合料重量60-70倍的去离子水中,超声5-10分钟,与上述复合硅烷溶液混合,送入到反应釜中,控制反应釜压力为0.9-1mpa,升高温度为90-95℃,保温搅拌1-2小时,出料冷却,离心分离,将沉淀干燥,得有机改性碳酸钙;
(4)取聚四氟乙烯蜡,加入到溶剂中,搅拌均匀,得蜡溶剂;
(5)取叔丁基对二苯酚,加入到其重量7-10倍的氯仿中,搅拌均匀,加入掺杂剂,超声10-20分钟,加入苯胺,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为65-70℃,加入上述引发剂水溶液,保温搅拌4-5小时,出料冷却,得聚苯胺溶液;
(6)取上述有机改性碳酸钙,加入到上述聚苯胺溶液中,搅拌均匀,加入三丁基三氯化锡,在80-90℃下保温搅拌30-40分钟,抽滤,将滤饼水洗,常温干燥,得改性聚苯胺;
(7)取上述改性聚苯胺,加入到蜡溶剂中,搅拌均匀,旋涂成膜,即得所述聚苯胺导电薄膜。
本发明的优点:
本发明首先采用硬脂酸处理轻质碳酸钙,通过硬脂酸的表面吸附作用来改善轻质碳酸钙表面的反应活性,然后与硅烷偶联剂分散处理的乙醇、十二烷基硫醇的共混,通过高温酯化,从而改善了碳酸钙在有机聚合物间的分散相容性,对于提高聚苯胺成品薄膜的力学稳定性起到了很好促进效果;
本发明在苯胺聚合过程中引入了酸掺杂剂,能够有效的提高聚苯胺成品的导电稳定性,同时加入的叔丁基对二苯酚则能够提高聚苯胺导电薄膜的贮存稳定性,本发明通过在溶剂中加入聚四氟乙烯蜡,可以有效的改善成品薄膜的抗张强度,同时促进各原料间的复合强度。
具体实施方式
下面结合实施例对本发明做进一步地描述。
实施例1
一种聚苯胺导电薄膜,按重量份数计,称取各原料:
硬脂酸4份、苯胺140份、过硫酸钠5份、十二烷基硫醇2份、对甲基苯磺酸2份、三丁基三氯化锡0.5份、溶剂200份、叔丁基对二苯酚1份、轻质碳酸钙8份、聚四氟乙烯蜡3份、硅烷偶联剂kh560 1份。
所述的溶剂为体积比为1:7的丙酮与二甲基甲酰胺的混合溶液。
该聚苯胺导电薄膜具体由包括以下步骤而制得:
(1)取过硫酸钠,加入到其重量30倍的去离子水中,搅拌均匀,得引发剂水溶液;
(2)取硅烷偶联剂kh560,加入到其重量13倍的无水乙醇中,升高温度为60℃,加入十二烷基硫醇,保温搅拌20分钟,得复合硅烷溶液;
(3)取硬脂酸,加热熔化,与轻质碳酸钙混合,加入到混合料重量70倍的去离子水中,超声10分钟,与上述复合硅烷溶液混合,送入到反应釜中,控制反应釜压力为1mpa,升高温度为95℃,保温搅拌2小时,出料冷却,离心分离,将沉淀干燥,得有机改性碳酸钙;
(4)取聚四氟乙烯蜡,加入到溶剂中,搅拌均匀,得蜡溶剂;
(5)取叔丁基对二苯酚,加入到其重量10倍的氯仿中,搅拌均匀,加入对甲基苯磺酸,超声20分钟,加入苯胺,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为70℃,加入上述过硫酸钠水溶液,保温搅拌5小时,出料冷却,得聚苯胺溶液;
(6)取上述有机改性碳酸钙,加入到上述聚苯胺溶液中,搅拌均匀,加入三丁基三氯化锡,在90℃下保温搅拌40分钟,抽滤,将滤饼水洗,常温干燥,得改性聚苯胺;
(7)取上述改性聚苯胺,加入到蜡溶剂中,搅拌均匀,旋涂成膜,即得所述聚苯胺导电薄膜。
实施例2
一种聚苯胺导电薄膜,按重量份数计,称取各原料:
硬脂酸3份、苯胺120份、过硫酸铵3份、十二烷基硫醇1份、柠檬酸1份、三丁基三氯化锡0.3份、溶剂170份、叔丁基对二苯酚0.8份、轻质碳酸钙6份、聚四氟乙烯蜡2份、硅烷偶联剂kh560 0.7份。
所述的溶剂为体积比为1:5的丙酮与二甲基甲酰胺的混合溶液。
该聚苯胺导电薄膜具体由包括以下步骤而制得:
(1)取过硫酸铵,加入到其重量25倍的去离子水中,搅拌均匀,得引发剂水溶液;
(2)取硅烷偶联剂kh560,加入到其重量10倍的无水乙醇中,升高温度为55℃,加入十二烷基硫醇,保温搅拌4分钟,得复合硅烷溶液;
(3)取硬脂酸,加热熔化,与轻质碳酸钙混合,加入到混合料重量60倍的去离子水中,超声5分钟,与上述复合硅烷溶液混合,送入到反应釜中,控制反应釜压力为0.9mpa,升高温度为90℃,保温搅拌1小时,出料冷却,离心分离,将沉淀干燥,得有机改性碳酸钙;
(4)取聚四氟乙烯蜡,加入到溶剂中,搅拌均匀,得蜡溶剂;
(5)取叔丁基对二苯酚,加入到其重量7倍的氯仿中,搅拌均匀,加入柠檬酸,超声10分钟,加入苯胺,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为65℃,加入上述过硫酸铵水溶液,保温搅拌4-5小时,出料冷却,得聚苯胺溶液;
(6)取上述有机改性碳酸钙,加入到上述聚苯胺溶液中,搅拌均匀,加入三丁基三氯化锡,在80℃下保温搅拌30分钟,抽滤,将滤饼水洗,常温干燥,得改性聚苯胺;
(7)取上述改性聚苯胺,加入到蜡溶剂中,搅拌均匀,旋涂成膜,即得所述聚苯胺导电薄膜。
性能测试:
实施例1的聚苯胺导电薄膜:
厚度1.6mm;
拉伸强度10.2Mpa;
电导率采用四探针法进行测试,结果为 0.80S/cm;
实施例2的聚苯胺导电薄膜:
厚度1.7mm;
拉伸强度11.3Mpa;
电导率采用四探针法进行测试,结果为 0.86S/cm。

Claims (5)

1.一种聚苯胺导电薄膜,其特征在于:它是由下述重量份的原料制成的:
硬脂酸3-4份、苯胺120-140份、引发剂3-5份、十二烷基硫醇1-2份、掺杂剂1-2份、三丁基三氯化锡0.3-0.5份、溶剂170-200份、叔丁基对二苯酚0.8-1份、轻质碳酸钙6-8份、聚四氟乙烯蜡2-3份、硅烷偶联剂kh560 0.7-1份。
2.根据权利要求1所述的一种聚苯胺导电薄膜,其特征在于:所述的掺杂剂选自对甲基苯磺酸或柠檬酸中的一种。
3.根据权利要求1所述的一种聚苯胺导电薄膜,其特征在于:所述的引发剂选自过硫酸铵、过硫酸钾或过硫酸钠中的一种。
4.根据权利要求1所述的一种聚苯胺导电薄膜,其特征在于:所述的溶剂为体积比为1:5-7的丙酮与二甲基甲酰胺的混合溶液。
5.根据权利要求1所述的一种聚苯胺导电薄膜,其特征在于:该聚苯胺导电薄膜由包括以下步骤制得: (1)取引发剂,加入到其重量25-30倍的去离子水中,搅拌均匀,得引发剂水溶液;
(2)取硅烷偶联剂kh560,加入到其重量10-13倍的无水乙醇中,升高温度为55-60℃,加入十二烷基硫醇,保温搅拌4-20分钟,得复合硅烷溶液;
(3)取硬脂酸,加热熔化,与轻质碳酸钙混合,加入到混合料重量60-70倍的去离子水中,超声5-10分钟,与上述复合硅烷溶液混合,送入到反应釜中,控制反应釜压力为0.9-1mpa,升高温度为90-95℃,保温搅拌1-2小时,出料冷却,离心分离,将沉淀干燥,得有机改性碳酸钙;
(4)取聚四氟乙烯蜡,加入到溶剂中,搅拌均匀,得蜡溶剂;
(5)取叔丁基对二苯酚,加入到其重量7-10倍的氯仿中,搅拌均匀,加入掺杂剂,超声10-20分钟,加入苯胺,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为65-70℃,加入上述引发剂水溶液,保温搅拌4-5小时,出料冷却,得聚苯胺溶液;
(6)取上述有机改性碳酸钙,加入到上述聚苯胺溶液中,搅拌均匀,加入三丁基三氯化锡,在80-90℃下保温搅拌30-40分钟,抽滤,将滤饼水洗,常温干燥,得改性聚苯胺;
(7)取上述改性聚苯胺,加入到蜡溶剂中,搅拌均匀,旋涂成膜,即得所述聚苯胺导电薄膜。
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