To increase the activity of immobilized catalyst by synergetic effect of adsorption and to extend the activity of Fe-0, a composite membrane with Fe-0, activated carbon fiber (ACF) and TiO2 was prepared, using dip-coating, impregnation and chemical reduction methods. The activity of the prepared membrane was evaluated for mineralizing 2,4-dichlorophenol (2,4DCP) in water under UV illumination. The co-presence of Fe-0 and TiO2 enhanced 2,4DCP degradation. ACF addition and its adsorption effect were shown in promoting 2,4DCP mineralization and TOC removal by comparing activities of composite membranes with Fe-0/TiO2/ACF or Fe-0/TiO2. Effects of pH and iron loading ratio to TiO2 on degradation rate of 2,4DCP using the composite membrane were investigated and optimized. The optimal pH was 6 and the optimal loading of Fe-0 was 1 wt% to TiO2. The repeated test results and XRD patterns of catalysts before and after reaction proved that the Fe-0/TiO2/ACF membrane was durable and stable in its photocatalytic activity. (C) 2009 Elsevier B.V. All rights reserved.