化工新型材料

化工新型材料 ›› 2018, Vol. 46 ›› Issue (4) : 98-103.

新材料与新技术

多壁碳纳米管的表面磺基化修饰

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Surface modification of multi walled carbon nanotube by sulfonic group

Shan Yingjie¹, Qiu Li¹, Hu Yafei¹, Li Sha², Chen Yongkang³, Liu Xuguang^1,3

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Received		Published
2017-01-09		2018-04-20
Issue Date	Revised Date
2018-05-17	2017-01-09

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摘要

用H₂SO₄与HNO₃(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。

Abstract

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

Key words

multi-walled carbon nanotube / sulfanilic acid / sulfonate / modification

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多壁碳纳米管的表面磺基化修饰[J]. 化工新型材料, 2018, 46(4): 98-103 DOI:

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