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Nitrogen-rich graphitized carbon microspheres(NGCs)with hierarchically porous were con-structed by self-assembly.Under different heat treatment conditions,the structure,mor-phology and properties of NGCs were studied by using multiple characterization techniques.The results showed that the chemical microenvironments(e.g.surface chemistry,degree of graphitization and defective,etc.)and microstructures properties(e.g.morphology,spe-cific surface area,particle size,etc.)could be delicately controlled via thermal carboniza-tion processes.The degradation of ofloxacin(OFLX)by NGCs activated peroxymonosulfate(PMS)was studied systematically.It was found that the synergistic coupling effect between optimum N or O bonding species configuration ratio(graphitic N and C=0)and special mi-crostructure was the main reason for the enhanced catalytic activity of NGC-800(calcina-tion temperature at 800℃).Electron paramagnetic resonance(EPR)experiments and rad-ical quenching experiments indicated that the hydroxyl(·OH),sulfate(S04·-)and singlet oxygen(102)were contributors in the NGC-800/PMS systems.Further investigation of the durability of chemical structures and surface active sites revealed that undergo N bond-ing species configuration reconstruction and cannibalistic oxidation during PMS activation reaction.The used NGC-800 physicochemical properties could be recovered by heat treat-ment to achieve the ideal catalytic performance.The findings proposed a valuable insight for catalytic performance and controllable design of construction.