Copper oxide (CuO) nanoparticles were synthesized by sonochemical technique using copper nitrate trihydrate and ammonium carbonate as precursors in the presence of polyethylene glycol (PEG). The reagents aqueous solution are exposed to ultrasound at different ultrasound power of 44, 66, 88, 110, and 132 W. The precipitated product was calcined at the temperatures of 4008C, 5008C, 6008C, and 7008C. The size, structure, and morphology of calcined CuO nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and energydispersive X-ray spectroscopy (EDAX). From the XRD observation, it is evident that the high purity CuO nanoparticles ranging from approximately 14 to approximately 54 nm were obtained. Additionally, SEM and EDAX investigation revealed that its structure and particle size are strongly dependent on the calcination temperature than ultrasound power. Most of the CuO nanoparticles formed were spherical in shape. Further, the application of the synthesized CuO nanoparticles toward the treatment of textile organic dyes such as Reactive Black 5 and Basic Blue 3 showed the synthesized CuO was highly effective in degradation of the environmental pollutants.