The application of nano-TiO2 as adsorbent combined with ultrasound for the degradation of N-acetyl-para-aminophenol (AAP) from aqueous solution was investigated. The nano-TiO2 was characterized by means of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), and attenuated total reflection–Fourier transform infrared spectroscopy (ATR-FTIR). Experimental results revealed that the adsorption of AAP by nano-TiO2 fitted the pseudo-second-order kinetic model, the equilibrium could be explained by the Freundlich isotherm and the treatment process is exothermic. The optimum removal efficiency of AAP (128.89 mg/g (77.33%)) was achieved at pH 4 when 0.03 g of nano-TiO2 was mixed with 50 mL of 100 mg/L AAP aqueous solution at ambient temperature, 60 min contact time, and a stirring speed of 120 rpm. Ultrasound at 20 kHz and pH 3 was favorable and it resulted in 52.61% and 57.43% removal efficiency with and without the addition of nano-TiO2, respectively. The degradation of AAP by ultrasound followed by nano-TiO2 treatment resulted in approximately 99.50% removal efficiency. This study showed that a sequential ultrasound and nano-TiO2 treatment process could be employed for the removal of AAP or other emerging water and wastewater contaminants.