摘要
采用化学氧化聚合法,以氯仿为溶剂、无水氯化铁为氧化剂,制得了聚噻吩样品,使用傅里叶变换红外光谱仪、紫外可见漫反射光谱仪和高阻计对样品结构和电导率进行了分析测试,考察了噻吩浓度(0.05~0.20mol/L)、反应时间(1~12h)、反应温度(-32~0℃)、氧化剂与噻吩摩尔比(2~5)、后处理方式对聚噻吩样品电导率的影响。研究表明:上述条件均会影响聚噻吩的聚合程度和连接方式,进而影响其电导率。当噻吩浓度由0.05mol/L增至0.20mol/L时,样品电导率从10^(-13) S/m降至10^(-8) S/m;反应时间为3h所得样品的电导率最大,为10^(-10) S/m;当反应温度在0^-32℃时,其电导率均在10^(-13) S/m数量级;氧化剂与噻吩摩尔比n(FeCl_3)/n(Th)的增大会使其电导率增加(10^(-13)~10^(-10) S/m);反应结束后直接对反应物进行过滤洗涤得到的样品比室温挥发完溶剂再洗涤得到样品的电导率高五个数量级。综合聚噻吩的电导率和原料成本,选定噻吩浓度为0.10mol/L、反应时间为3h、反应温度为0℃、n(FeCl_3)/n(Th)=2,对反应物直接过滤洗涤为最佳制备条件,该条件下所得聚噻吩样品的电导率高达2.49×10^(-8) S/m。
Polythiophenes were prepared by chemical oxidative polymerization under the conditions of different reaction time t（1~12h）,temperatureθ（-32~0 ℃）,molar ratio of oxidant to thiophene n（FeCl_3）/n（Th）= 2~5,thiophene concentration c（Th）=0.05~0.20mol/L.The structure and conductivity of the polythiophenes were characterized using Fourier transform infrared spectroscopy,ultraviolet and visible diffuse reflectance spectroscopy and megohmmeter.The results indicate that these preparation conditions could greatly affect the structure and conductivity of polythiophenes.The conductivity of polythiophene increase from 10^（-13） to 10^（-8） S/m with the increase of thiophene concentration from 0.05 to 0.20mol/L.The highest conductivity of polythiophene at different reaction time is 10^（-10） S/m when the reaction time is 3h.The conductivity of the polythiophenes prepared at different temperatures is all at 10^（-13） S/m level.When the n（FeCl_3）/n（Th）increases from 2 to 5,the conductivity of samples increases from 10^（-13） to 10^（-10） S/m.The conductivity of the sample prepared by the treatment of direct filtration and washing increases 5 orders of magnitude over that prepared by the treatment of solvent volatilization at room temperature followed by filtration and washing.From the aspect of the balance of conductivity and cost,the optimized reaction conditions are：c（Th）=0.1mol/L,t=3h,θ=0 ℃,n（FeCl_3）/n（Th）=2,and using direct filtration treatment on the products.Moreover,the optimized conductivity of the polythiophene is 2.49×10^（-8） S/m.
作者
王亚杉
廖俊杰
韩鹏月
常丽萍
鲍卫仁
WANG Yashan LIAO Junjie HAN Pengyue CHANG Liping BAO Weiren(State Key Laboratory Breeding Base of Coal Science and Technology Co-founded by Shanxi Province and Ministry of Science and Technology, Taiyuan University of Technology, Taiyuan 030024, Chin)
出处
《太原理工大学学报》
北大核心
2017年第4期563-569,共7页
Journal of Taiyuan University of Technology
基金
国家自然科学基金资助项目:吸附剂表面修饰和结构调变对焦化苯中噻吩深度脱除的影响及其再利用研究(51372161)
吸附剂的表面化学特性对深度脱除汽油中噻吩类含硫化合物的影响及吸附机理研究(21406151)
关键词
化学氧化聚合法
聚噻吩
电导率
聚合度
连接方式
chemical oxidative polymerization
polythiophene
conductivity
degree of polymerization
connection manner of thiophene
