A series of Fe(II)/meso-Al2O3 catalysts was prepared by the wetness impregnation method using ferrous sulfate and mesoporous alumina. Mesoporous alumina was synthesized at pH 6 by the precipitation method using aluminum isopropoxide as the aluminum source and sucrose as the template. These catalysts were characterized by different techniques such as SEM, XRD, XPS, FTIR spectroscopy, and BET surface area analysis. The catalytic activities in phenol degradation by the photo-Fenton reaction were evaluated. The effects of H2O2 concentration, pH, and additive (ethanol) on the photo-Fenton reaction were studied. The sample with 0.25 wt % Fe(II)/meso-Al2O3-6 was found to be an efficient catalyst, showing 98% degradation of 2.1 x 10(-5) mol of phenol at pH 6 in 1 h.