多壁碳纳米管的表面磺基化修饰  

Surface modification of multi walled carbon nanotube by sulfonic group

作　　者：单英杰[1] 邱丽[1] 胡雅菲 李莎 陈永康[3] 刘旭光[1,3] Shan Yingjie;Qiu Li;Hu Yafei;Li Sha;Chen Yongkang;Liu Xuguang(College of Chemistry and Chemieal Engineering,Taiyuan University of Technology, Taiyuan 030024;College of Textile Engineering, Taiyuan University of Technology, Taiyuan 030024;Key Laboratory of Interface Science and Engineering in Advanced Materials, Ministry Education, Taiyuan 030024)

机构地区：[1]太原理工大学化学化工学院,太原030024 [2]太原理工大学轻纺工程学院,太原030024 [3]太原理工大学新材料界面科学与工程教育部重点实验室,太原030024

出　　处：《化工新型材料》2018年第4期98-103,共6页New Chemical Materials

基　　金：山西省基金(201601D202018;201601D202019);山西省国际科技合作项目(2015081045)

摘　　要：用H_2SO_4与HNO_3(体积比为3∶1)的混酸对原始多壁碳纳米管(p-MWCNTs)进行修饰,使p-MWCNTs表面氧化生成酸化多壁碳纳米管(a-MWCNTs);通过N,N′-二环己基碳二胺(DCC)缩合作用,使对氨苯磺酸的氨基与a-MWCNTs表面羧基缩合脱水得到磺化多壁碳纳米管(s-MWCNTs)。采用热压成型法在聚醚醚酮(PEEK)基体中分别加入不同改性的多壁碳纳米管(MWCNTs)制得MWCNTs/PEEK复合材料。在磺化过程中研究了DCC用量、反应时间和对氨基苯磺酸用量对s-MWCNTs表面接枝率的影响。采用热重分析、场发射电子显微镜、红外和拉曼光谱对不同改性MWCNTs进行形貌和结构分析。结果表明,在a-MWCNTs用量为0.3g,DCC用量为0.5g、反应时间为6h和对氨基苯磺酸用量为0.3g条件下,所得s-MWCNTs之间堆积松散,分散性较好,失重率最大。动态力学分析表明,s-MWCNTs/PEEK复合材料的储能模量显著增加。Multi-walled carbon nanotubes （MWCNTs） were oxidized by a mixture of concentrated sulfuric acid and nitric acid （volume ratio of 3：1） to improve their surface activity, resulting in the formation of carboxyl groups on their surfaces.Then,the oxidized MWCNTs reacted with sulfanilic acid to prepare sulfonated MWCNTs with N, N＇ dicyclohexyl carbodiimide （DCC） as condensation agent by forming amido bond.The influences of DCC dosage,reaction time and sulfanilic acid dosage were studied. The morphology and structure of the products were characterized by thermogravimetry, field emission scanning electron microscopy, Fourier transformation infrared spectrometry and Raman spectra.The results showed that the preferable optimized factors of DCC dosage, reaction time and sulfanilic acid dosage were 0.5g,6h,0.3g for 0.3g of oxidized MWCNTs respectively.The characteristic peak of sulfonic acid group was observed in the surface of s-MWCNTs, MWCNTs stacked loosely and dispersed well.Meanwhile, weightlessness of MWCNTs was maximum.Dynamic mechanical analysis demonstrated that improvement of storage modulus was even higher at the same level of s-MWCNTs in the MWCNTs/PEEK composite.

关 键 词：多壁碳纳米管 对氨基苯磺酸 磺化 修饰 

分 类 号：O613.71[理学—无机化学] TB306[理学—化学] TB383.1[一般工业技术—材料科学与工程]