节点文献
内嵌金属钇富勒烯的制备、分离与结构
【作者】 梁希慧；
【导师】 廉永福；
【作者基本信息】 黑龙江大学 ， 分析化学， 2012， 硕士
【摘要】 内嵌金属富勒烯的物理化学性质，分子电子性质，几何结构等与空心富勒烯有很大不同。由于其结构新奇美观、性质奇特，内嵌金属富勒烯在光学、磁学、分子电子器件及生物医学工程等诸多高科技领域有广阔的应用前景。然而由于内嵌金属富勒烯产率低、种类多、分离困难等而限制了广泛深入的研究。本论文首先，采用传统的电弧放电法对钇源进行选择；其次，使用四种烟炱前处理方法对提取方法进行选择；再次，通过柱色谱富集实验富集大量内嵌金属富勒烯样品，进一步缩短内嵌金属钇富勒烯的分离时间，提高分离效率；最后通过多步高效液相色谱分离、MS、Vis-NIR、CV和13CNMR检测，得到纯度很高（>95%）的多种内嵌金属钇富勒烯：Y2C82（Ⅰ、Ⅲ），Y2C84（Ⅰ、Ⅲ），Y2C90（Ⅰ），Y2C92（Ⅰ、Ⅱ）和Y@C82，并确定Y2C2@C82（Ⅲ）和Y2@C82（Ⅲ）的分子结构同属C82-C3v（8）。
【Abstract】 Endohedral Metallofullerenes (EMFs) which are different from fullerenes in various properties such as chemical and physical properties, molecule and electrical properties, electronic structures, have a wide range of potential applications in photoelectrochemical materials, magnetic resonance imaging contrast agents, and medical diagnosis. Because of the low yields, various species (e.g., various metals, cage sizes, and symmetries) and difficult purification, these attractive molecules are also not widely or deeply researched.In this paper, we prepare the soot by classic DC arc discharge with various sources of yttrium, isolate the soot by means of four diverse treatments, and with the help of column chromatographic isolation, we enrich a great quantity of yttrium metallofullerenes. Finally, a series of Y metallofullerenes based on different fullerene cages, i.e. Y2C80(I), Y2C82(I, III), Y2C84(I, III), Y2C90(I), Y2C92(I, II) and Y@C82are successfully isolated by multi-steps HPLC, and we also confirm that the structure of Y2@C82(IIII) is exactly the same as that of Y2C2@C82(III), i.e. C82-C3v (8), detected by MS, Vis-NIR, CV,13C NMR.