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In this work, the MoS2–RGO nanocomposites were successfully prepared by a lithiation assisted exfoliation method and analyzed by various spectroscopic techniques such as X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), and Raman spectroscopy. The sonocatalytic performance in the degradation of methylene blue (MB) under ultrasonic irradiation was investigated. The complete degradation of MB was achieved using sonocatalyst–MoS2–RGO nanocomposites, while restacked MoS2 show lower sonocatalytic performance. This excellent sonocatalytic activity was due to the synergistic effect of the MoS2 and RGO. Our finding revealed that the MoS2–RGO nanocomposites were an active catalyst for the sonocatalytic degradation of dyes. Besides, the cycling tests indicated that the MoS2–RGO composite exhibited excellent stability. The fabricated composite could be effectively utilized for various environmental remediation applications. [ABSTRACT FROM AUTHOR]