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In this work, nano-sized mixed oxides of Mn3O4 and CuO were successfully prepared by a simple hydrothermal method and used as an effective heterogeneous sono-Fenton catalyst for p-nitrophenol (PNP) degradation at the neutral condition. The prepared nanocomposite was characterised by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) and N2 adsorption–desorption analysis. The results showed that the Mn3O4.CuO nanocomposite can catalyze efficiently the decomposition of PNP under ultrasonic irradiation in comparison with pristine Mn3O4 and CuO. The almost complete degradation of PNP was achieved within 20 min at pH 8.0 by using 0.1 mol/L of H2O2 and 0.01 g of the catalyst. Also, the stability and reusability test showed that the prepared nanocomposite had good stability during the Fenton process. Finally, the main oxidative species involved in the sono-Fenton process based on the results of radical species trapping experiments were identified.