Proper treatment of hazardous contaminants in the air, land, and water is crucial to environmental remediation. Sonocatalysis, by using ultrasound and suitable catalysts, has shown its potential in organic pollutant removal. In this work, K3PMo12O40/WO3sonocatalysts were fabricatedviaa facile solution method at room temperature. Techniques such as powder X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, and X-ray photoelectron spectroscopy were used to characterize the structure and morphology of the products. By using the K3PMo12O40/WO3sonocatalyst, an ultrasound-assisted advanced oxidation process has been developed for the catalytic degradation of methyl orange and acid red 88. Almost all dyes were degraded within 120 min of ultrasound baths, proving that the K3PMo12O40/WO3sonocatalyst has the advantage of speeding up the decomposition of contaminants. The impacts of key parameters, including catalyst dosage, dye concentration, dye pH, and ultrasonic power were evaluated to understand and reach optimized conditions in sonocatalysis. The remarkable performance of K3PMo12O40/WO3in the sonocatalytic degradation of pollutants provides a new strategy for the application of K3PMo12O40in sonocatalysis.