Ten-gram Preparation Method And Electrochemical Performance Of Nitrogen-doped Ordered Mesoporous Carbon Nanospheres

Mesoporous carbon materials have potential applications in some fields such as adsorption separation and drug sustained-release due to their special porous structure and high surface area. After doping heteroatom into the framework of mesoporous carbon as catalysis active sites, the resultant materials can be used as catalyst, and applied in the reaction of oxygen reduction. As far as the atomic species, doping nitrogen atom is one of research hotspots in field of material design. Compared with unordered porous structure, nitrogen doped ordered mesoporous carbon material has higher specific surface area and more unblocked channel, which is beneficial for increasing the catalysis reaction rate. Therefore, extensive research has pay attention on how to efficiently dope nitrogen into the framework of carbon materials and how to accurately distinguish the bonding type of nitrogen. There are few researches on the morphology controlled synthesis of nitrogen doped mesoporous carbon materials. It is known that the morphology of materials has influence on their properties, and thus developing the facile and morphology controlled preparation method is desired.On the basis of literatures,20 g scalable preparation of nitrogen doped ordered mesoporous carbon nanospheres is realized by using F127 as template and 3-amino phenol as carbon source after optimizing preparation parameters. In addition, their electrochemical supercapcitve properties are preliminarily investigated. Finally, the method of efficiently loading metal oxides nanoparticles on them is explored. These researches are valuable for wildly application of this material in the modern industry.The detail contents and results are as follows.(1)Under the conditions of F127 as template and 3-aminophenol as carbon source, the influences of preparation parameters, such as the type of carbon source, ratio of H2O/ethanol, dosage of surfactant, reaction temperature, stirred time and so on, on the morphology, dimension size distribution and ordered level of nitrogen doped ordered carbon materials are studied. And then, in the scalable system, the effects of parameters such as the type of carbon source and dosage of NH3·H2O on the formation of spherical morphology and ordered porous structure are investigated. Further, the correlation between carbonization temperature and graphitization degree and the maintenance of porous structure is researched.Some valuable results are obtained. The resultant products have ordered mesoporous structure, high surface areas of 434.8-572.07 m2g-1 and large pore volume of 0.2-0.283cm3g-1. The pore size distribution is narrow and centers at 2.3?4.5nm and 4.6 nm. After different temperature carbonization, the material has good electrochemical super capacitive properties, at 0.5A/g conditions, specific capacitance can reach 198.9F/g.In the framework of the products four types of nitrogen exist, and they are pyridine type, pyrrole type, Graphite type and oxidized type, respectively. It is found that the optimized carbonization temperature is 600?, which is helpful for improving the degree of ordered porous structure and graphitization. An optimized experiment condition is obtained, under which 20 g product can be prepared in one batch.(2)The method of loading CoO nanoparticles on the support of nitrogen doped ordered mesoporous carbon nanospheres is explored. More attentions are paid on the influence of experiment parameters, including the surface chemical properties of the support, the type and dosage of used metal slats, reaction time and type of dispersant, on the morphology and distribution of CoO nanoparticles.The results show that increasing the hydrophilicity and adding polyethylene glycol (PEG) as dispersant can effectively inhibit the aggregation of CoO nanoparticles and thus improve their dispersion on the support, and the size of CoO nanoparticles can be controlled less than 20 nm.