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Microwave-assisted covalent sidewall functionalization of multiwalled carbon nanotubes

机译:多壁碳纳米管的微波辅助共价侧壁官能化

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Thermal cycloaddition of 1,3-dipolar azomethine ylides to the side-walls of multiwalled carbon nanotubes (MWNTs) has been used to prepare MWNTs that contain 2-methylenethiol-4-(4-octadecyloxyphenyl) (4), N-octyl2-(4-octadecyloxyphenyl) (5) or 2-(4octadecyloxyphenyl)pyrrolidine (6) units. All these contain the 4-octadecyloxyphenyl substituent that acts as a solubilizing group. Microwave (MiW)-assisted heating was found to be highly efficient for soluble MWNTs, for which the amount of added groups after only 2 h of NEW heating at 200 degrees C, determined by using thermogravimetric analysis, was found to be in the same range as that obtained after 100-120 h of conventional heating of soluble and insoluble MWNTs. Solubility is a key feature for a successful MiW-heated reaction; MWNTs insoluble in the reaction medium yielded considerably less addends in the MiW-heated reactions than in the conventionally heated reaction. The location and even distribution of the pyrrolidine units over the outermost layer of the MWNTs was verified by transmission electron microscopy analysis of 4 that had been treated with,.,old nanoparticles and thoroughly washed to remove gold particles adsorbed on nonfunctionalized parts of the MWNTs.
机译:1,3-偶极偶氮甲亚胺基团在多壁碳纳米管(MWNTs)侧壁上的热环加成已用于制备包含2-亚甲基硫醇-4-(4-十八烷基氧苯基)(4),N-辛基2-( 4-十八烷基氧基苯基)(5)或2-(4-十八烷基氧基苯基)吡咯烷(6)单元。所有这些均含有作为增溶基团的4-十八烷基氧苯基取代基。发现微波(MiW)辅助加热对于可溶性MWNT非常有效,通过热重分析确定200℃的NEW加热仅2 h后,添加的基团数量在相同范围内与常规加热可溶性和不溶性MWNT 100-120小时后获得的结果相同。溶解度是成功进行MiW加热反应的关键特征。与常规加热的反应相比,不溶于反应介质的MWNT在MiW加热的反应中产生的加合物要少得多。吡咯烷单元在MWNTs最外层的位置和均匀分布已通过透射电子显微镜分析对4种用旧的纳米颗粒处理并彻底洗涤以除去吸附在MWNTs非功能化部分上的金颗粒进行了验证。

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