多壁碳纳米管的表面乙烯基功能化

Vinyl-functionalization of Multi-walled Carbon Nanotubes

本文采用浓硫酸浓硝酸(3∶1,v v)组成的混酸体系在140℃时对多壁碳纳米管进行了氧化处理,并通过氧化后在多壁碳纳米管表面生成的羟基官能团与丙烯酰氯进行反应,制备了表面乙烯基功能化的多壁碳纳米管。强酸氧化后多壁碳纳米管的表面形貌通过透射电子显微镜进行了观察,结果表明氧化时间为60分钟时所得多壁碳纳米管的长度比较均匀,长径比较大,具有明显的两端开口结构。氧化后多壁碳纳米管表面的官能团通过核磁共振波谱仪进行了表征,结果表明混酸氧化处理60分钟后的多壁碳纳米管的管壁和管端生成了羟基等官能团。氧化后的多壁碳纳米管与丙烯酰氯充分反应后的产物的核磁共振氢谱图表明,反应产物为乙烯基功能化的多壁碳纳米管。

Multi-walled carbon nanotubes （MWNTs） have been chemically oxidized and shortened using a mixture of concentrated sulfuric and concentrated nitric acids （3：1, v/v, 98% and 70%, respectively） at 140℃ under reflux. By the reaction of acryloyl chloride with hydroxyl groups present at the sidewall defect sites and the open ends of oxidized MWNTs, vinyl-functionalized MWNTs have been successfully prepared, Transmission electron microscopy （TEM） was used to measure the morphology of oxidized MWNTs, and the obtained results indicated that the oxidization time of 60 min was optimum since at that time oxidized MWNTs with the open ends were obtained, and their length diameter ratio was very large, By characterization and analysis of the oxidized MWNTs at the oxidization time of 60 min using proton nuclear resonance spectroscopy （ HNMR ）, it was found that acid-oxidization of MWNTs produced hydroxyl groups present at the sidewalls and the open ends of oxidized MWNTs. The HNMR data of the products resulted from the reaction of oxidized MWNTs at the oxidization time of 60 min with acryloyl chloride confirmed that they were vinyl-functionalized MWNTs。