NiS-clinoptilolite is prepared by ion exchange and precipitation procedures and is characterized by Fourier transformation infrared, X-ray diffraction, thermal analysis, SEM and BET methods. The prepared composite is used as a catalyst for photodegradation of furfural in aqueous solution under UV irradiation. The degradation process is monitored during the experimental runs by UV/Vis absorption, COD and TOC concentration determination and HPLC methods. The effect of key operating parameters such as catalyst dosage, initial concentration of furfural, initial pH of the solutions and effect of the presence of hydrogen peroxide and potassium bromate is studied on the degradation efficiency. The optimal operation parameters are found as follows: pH 5, 330 mg L-1 of the catalyst loading and 6 mM of furfural concentration. It observed that the degradation rate increased with an increasing mass of hydrogen peroxide and potassium bromate. The NiS particles out of the zeolite framework did not show significant degradation efficiency. (C) 2011 Elsevier B.V. All rights reserved.