In the present study, the ultrasound in pulsed mode was used as a part of an advanced oxidation method. The influence of the pulsed ultrasound mode for the preparation of the zinc oxide (ZnO) wurtzite nanoparticle was investigated. The catalysts synthesized were analysed using SEM, TEM, EDAX, BET surface area, XRD, and DRS to study their morphological and structural characterizations. The ZnO nanoparticles exhibited a highly hexagonal structure from pulsed sonication synthesis route. The efficiency of the decolourization of the reactive red 4 (RR4) dye was studied under different operation parameters such as dye concentration, initial solution pH, oxidant (e.g., H2O2) concentration, and catalyst loading. The hybrid combined process of pulsed sonolysis, pH (4.0), H2O2 (17.64 mmol), and catalyst (0.35 g/L) achieved 97% degradation and 87.5% chemical oxygen demand removal in about 20 min of reaction time. The cyclic degradation studies of RR4 removal with 0.35 g/L of ZnO showed the reusability of catalyst up to the fifth removal cycle with negligible loss in the catalytic performance. GC–MS study, used for the detection of the RR4 intermediates, revealed the oxidation–reduction reaction by the reactive radicals proceeded via the reductive cleavage of the azo bonds. The studied process, based on the pulsed ultrasound, is found to be effective for the degradation of RR4 dye.