The removal process of NO from SO2-containing simulated flue gas using an ultraviolet (UV)/Fenton-like reaction in a photochemical reactor was investigated. The effects of several operating parameters, such as the H2O2 concentration, Cu2+ concentration, solution pH, NO concentration, solution temperature, gas flow, SO2 concentration, and O-2 concentration on NO removal were studied using a single-factor method. The liquid anions were measured by ion chromatography, and the material balances for NO and SO2 were also calculated. The results show that, with the increase in the Cu2+ concentration, NO removal efficiency significantly increases. With the increase in the H2O2 concentration, NO removal efficiency increases, but the changes gradually become smaller. NO removal efficiency greatly reduces with an increasing gas flow and NO concentration. An increasing solution temperature or SO2 concentration slightly decreases NO removal efficiency. An increase in the O-2 concentration can promote the removal of NO. The anions in the liquid phase are mainly SO42- and NO3-. The calculated values of SO42- and NO3- are overall in agreement with the measured values.