TiO/Montmorillonite (TiO/MMT) nanocomposite as sonocatalyst was produced by immobilizing synthesized TiO on the surface of montmorillonite. The characteristics of produced nanocomposite were investigated using XRD, XRF, FTIR, TEM, SEM, EDX, UV-vis DRS and nitrogen adsorption-desorption analyses. The synthesized TiO and TiO/MMT samples were applied as catalysts for sonocatalytic degradation of ciprofloxacin (CIP). The performance of the TiO/MMT was greater than pure TiO sample in treatment of CIP solution. The degradation efficiency of the CIP by sonocatalytic process was affected by solution pH, catalyst dosage, initial CIP concentrations and ultrasonic power. Degradation efficiency of 65.01% was obtained at the pH of 6, catalyst dosage of 0.2gL, initial CIP concentration of 10mgL and ultrasonic power of 650WL. It was observed that the presence of inorganic and organic scavengers suppressed the performance of sonocatalytic process. The stability of the nanocomposite was studied in several successive experiments, and the degradation efficiency declined only 61.48% after 4 repeated experiments. The main degradation by-products were recognized by GC-MS method to propose the possible sonocatalytic mechanism for the degradation of CIP.