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煤基富勒烯(C60)的制备与提纯

PREPARATION AND PURIFICATION OF FULLERENES FROM METALLURGICAL COKE

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【作者】 邱介山周颖张红兵罗长齐周红艺

【Author】 Qiu Jieshan,Zhou Ying, Zhang Hongbing and Luo Changqi(Institute of Chemical Engineering, Dalian University of Technology, Dalian 116012)Zhou Hongyi(College of Technical and Vocational Education ,Zhejiang University of Technology,Hangzhau 310014)

【机构】 大连理工大学化工学院浙江工业大学职业技术教育学院 大连116012大连116012杭州310014

【摘要】 <正>富勒烯是除石墨和金刚石外碳的第三种同素异构体,其代表性分子是C60和C70。大量研究成果表明,富勒烯的特殊球形空心分子结构赋予了它许多奇异的物理化学性质,在超导、非线性光学、催化剂等诸多领域显示出十分诱人的应用前景。目前,国内外主要以高纯石墨电极为原料制备富勒烯,由于煤的价格低廉且来源广泛,以煤炭为原料制备富勒烯的研究备受国外学者的关注。本文以冶金焦为原料用电弧法制备富勒烯,研究了实验操作条件及冶金焦性质与富勒烯收率间的关系。粗富勒烯以活性炭为固定相,甲苯为流动相的柱色谱分离提纯,考察了活性炭的孔隙结构及柱色谱的长度对C60纯度和收率的影响。

【Abstract】 Fullerene has been prepared from four commercial cokes by electrical arcing in helium atmosphere and purified by column chromatography using activited carbons as the stationary phase. The crude and pure fullerene products are characterized by high pressure liquid chromatography, mass spectrometry and UV-Vis spectrometry. The results are discussed in terms of the carbon arc evaporation process parameters and the properties of coke. The yield of crude fullerenes decreased as the volatile matter content of coke increases and the composition of crude fullerenes depends on the volatile matter content of coke. After column chromatography separation with pure toluene as mobile phase on active carbon-silica gel, 99. 9% C60 is obtained. The yield of pure C60 is affected by the microstructure of active carbon and the length of column chromatography.

【关键词】 富勒烯冶金焦柱色谱提纯
【Key words】 fullerenemetallurgical cokecolumn chromatographypurification
【基金】 国家自然科学青年基金(No.29506041);辽宁省自然科学基金资助项目
  • 【文献出处】 化工学报 ,Journal of Chemical Industry and Engineering(China) , 编辑部邮箱 ,1997年02期
  • 【分类号】O613
  • 【被引频次】23
  • 【下载频次】352
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