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Novel mesoporous carbonaceous materials: Synthesis, characterization and applications in liquid chromatography

Posted on:2004-12-19Degree:Ph.DType:Dissertation
University:Kent State UniversityCandidate:Li, ZuojiangFull Text:PDF
GTID:1451390011957963Subject:Chemistry
Abstract/Summary:
The ability to control the porous structure in carbonaceous materials has been significantly improved in the past decade due to the appearance of new synthetic routes and novel templating materials. In this dissertation, novel mesoporous carbonaceous materials with controlled structural and surface properties were prepared and investigated using low temperature nitrogen adsorption, thermal analysis, X-ray diffraction and other analytical techniques. The performance of these novel mesoporous carbons in liquid chromatography was also investigated.; Carbons with extremely high mesoporosity were synthesized by using mesophase pitch and polyacrylonitrile as precursors in the silica gel templating method, which led to a dramatic reduction of microporosity and high carbonization yield. The most important achievement of this dissertation is the initiation of a colloidal imprinting technique, in which spherical pores were created in the particles of mesophase pitch by using silica colloids of proper size. This method allows us to prepare carbons with uniform spherical pores in the range of 7–70 nm and narrow pore size distribution, filling the pore size gap between carbons templated with ordered silicas and colloidal silica crystals. The introduction of air stabilization further improved the ability to control the pore development at a given stage in the imprinting process. For the first time, carbon particles with mesoporous shell/nonporous core structure were obtained. In this way, carbons with controlled pore size, surface area, pore volume and particle size were synthesized. Moreover, the colloidal imprinting technique was extended to a more general imprinting concept, in which porous particles were used to obtain carbon particles having ordered or disordered structure on their surface. Graphitization of the imprinted carbons provided carbonaceous materials of tailored mesopores and graphitic structure. Also, this high-temperature treatment removed surface functional groups and increased surface homogeneity. The graphitized carbons with surface mesoporosity showed a good separation efficiency in reverse phase high performance liquid chromatography due to their unique structure. In addition, these carbons showed a good selectivity to some polar solutes and quite different retention mechanism from that observed for octadecyl bonded phases.
Keywords/Search Tags:Carbonaceous materials, Novel mesoporous, Structure, Liquid, Carbons
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