化学学报 ›› 2012, Vol. 70 ›› Issue (07): 817-821 .DOI: 10.6023/A1112251    下一篇

研究论文

原子转移氮氧自由基偶合反应制备聚苯乙烯改性的石墨烯

陈小乙a,b, 石远琳a, 杨东a, 胡建华a, 杨芃原b   

  1. a 聚合物分子工程国家重点实验室 复旦大学高分子科学系 上海 200433;
    b 复旦大学化学系 上海 200433
  • 收稿日期:2011-12-25 修回日期:2012-02-06 出版日期:2012-04-14 发布日期:2012-02-15
  • 通讯作者: 杨东 E-mail:yangdong@fudan.edu.cn; hujh@fudan.edu.cn
  • 基金资助:

    国家自然科学基金(Nos. 50873029, 51073042, 51103026)、上海科技创新行动计划(No. 11JC1400600)、上海市自然科学基金(No. 11ZR1403100)和高等学校博士学科点专项科研基金(No. 20110071120006)资助项目.

Preparation of Polystyrene Functionalized Graphene by Atom Transfer Nitroxide Radical Coupling Reaction

Chen Xiaoyia,b, Shi Yuanlina, Yang Donga, Hu Jianhua, Yang Pengyuanb   

  1. a State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular Science, Fudan University, Shanghai 200433;
    b Department of Chemistry, Fudan University, Shanghai 200433
  • Received:2011-12-25 Revised:2012-02-06 Online:2012-04-14 Published:2012-02-15
  • Supported by:

    Project supported by the National Natural Science Foundation of China (Nos. 50873029, 51073042, 51103026), Shanghai Scientific and Technological Innovation Project (No. 11JC1400600), Shanghai Natural Science Funds (No. 11ZR1403100), and the Specialized Research Fund for the Doctoral Program of Higher Education (No. 20110071120006).

通过原子转移氮氧自由基偶合(ATNRC)反应制备了聚苯乙烯改性的石墨烯. 先将氧化石墨烯酰氯化, 然后与2,2,6,6-四甲基-4-羟基哌啶-1-氧自由基(HTEMPO)进行酯化反应制备HTEMPO 修饰的石墨烯(Graphene-HTEMPO), 通过Graphene-HTEMPO 与原子转移自由基聚合(ATRP)方法制备的Br 封端的聚苯乙烯进行ATNRC 反应, 即可得到聚苯乙烯共价改性的石墨烯(Graphene-g-PS). 热失重分析结果表明聚苯乙烯的接枝率约为6.68 wt%, 从透射电镜照片中也可以明显地看到石墨烯表面的聚苯乙烯. 由于聚苯乙烯的共价接枝, 使得Graphene-g-PS 在氯仿、正己烷、甲苯、甲醇等有机溶剂中具有很好的分散性, 有利于石墨烯的进一步应用.

关键词: 石墨烯, 聚苯乙烯, 原子转移氮氧自由基偶合反应, 化学改性

Polystyrene functionalized graphene was prepared by atom transfer nitroxide radical coupling (ATNRC) reaction. Graphene oxide was first reacted with thionyl chloride, followed by esterification with 4-hydroxy-2,2,6,6-tetramethyl-piperidinyl-1-oxyl (HTEMPO) to prepare HTEMPO functionalized graphene (Graphene-HTEMPO). Then, Graphene-HTEMPO was coupled with Br-end-capping polystyrene prepared by atom transfer radical polymerization (ATRP) via ATNRC reaction to obtain polystyrene covalently functionalized graphene (Graphene-g-PS). The thermogravimetric analysis result showed that the graft ratio of PS was 6.68 wt%. The PS on the surface of graphene could be obviously observed from the TEM image. Because of the covalent graft of PS, Graphene-g-PS showed good dispersibility in chloroform, hexane, toluene, methanol, etc., which is favorable to the further application of graphene.

Key words: graphene, polystyrene, atom transfer nitroxide radical coupling reaction, chemical functionalization