The nitroaromatic compounds, known as organic pollutants, have arising attention due to their carcinogenic character, highly dangerous to human health. In this work, the Ag@ZnO/MWCNT ternary nanocomposite synthesized via conjugation of sonochemical and solvothermal treatments manifests high performance in the reduction of 4-nitrophenol in the aqueous media (TOF value of 246 minmol metal). The incorporation of MWCNT onto the nanocomposite structure favored the reusing of the catalysts even after eight consecutive catalytic runs without catalysts cleaning nor product removal. Obtained samples were characterized by XRD, TEM, UV-vis, Raman and FTIR spectroscopies. It was found that ultrasonic treatment at relatively moderate conditions leads to functionalization of MWCNT, the appearance of C=C and OH groups and change of electronic properties of Ag@ZnO/MWCNT composite which provide its stable material dispersion in aqueous solution and high catalytic performance in the 4-nitrophenol reduction. This technique may be effectively applied for the functionalization of carbon including materials for their usage in an aqueous media.