A novel process on simultaneous removal of NO and SO2 using aqueous peroxymonosulfate (PMS) with synergic activation of Cu2+/Fe3+ and high temperature in an impinging stream reactor is developed for the first time. Effects of PMS concentration, Cu2+/Fe3+ concentration, reaction temperature, solution pH, flue gas flow, liquid-gas ratio, gas components, and inorganic ions on NO/SO2 removals were investigated. Active species and products were determined by electron spin resonance spectroscopy and ion chromatography. Removal pathways of NO/SO2 were revealed, and mass transfer-reaction kinetics of NO removal was studied. The optimal experimental conditions are obtained. H2SO4 and HNO3 are the main products. It is found that there is a clear synergy between Cu2+/Fe3+ and high temperature for activating PMS. SO4- and similar to OH are found to be the main oxidants for NO removal. NO removals belong to pseudo-first fast reactions in the two investigated oxidation systems. Besides, the kinetic parameters are also measured. (C) 2016 American Institute of Chemical Engineers AIChE J, 63: 1287-1302, 2017