In this investigation, nano ZnO was sonochemically synthesized by a novel method using a methionine precursor. A narrow size distribution (41-50 nm) of nano ZnO was achieved that was immobilized on perlite and applied as a catalyst in catalytic ozonation. The catalyst was characterized by fourier transform infrared spectroscopy, BET surface area, and field emission scanning electron microscope. The ozonation of recalcitrant Remazol black 5 (RB5) di-azo dye solution by means of the synthesized catalyst was investigated in a bubble column slurry reactor. The influence of pH values (7, 9, 11), catalyst dosage (8, 12, 15, 20 g L −1) and reaction time (10, 20, 30, 60 min) was investigated. Although the dye color was completely removed by single ozonation at a higher reaction time, the applied nanocatalyst improved the dye declorination kinetics. Also, the degradation of the hazardous aromatic fraction of the dye was enhanced five-times by catalytic ozonation at a low reaction time (10 min) and a neutral pH. The second-order kinetics was best fitted in terms of both RB5 color and its aromatic fraction removal. The total organic carbon analysis indicated a significant improvement in the mineralization of RB5 by catalytic ozonation using the nano-ZnO/perlite catalyst.