A series of novel Cu-incorporated mesoporous materials (CMMs) with molar ratios of Cu/Si ranging from 1/200 to 1/20 were synthesized by sol-gel method using glutaric acid as template. The materials were characterized by powder X-ray diffraction (XRD), N-2 adsorption, diffuse reflectance UV-vis spectroscopy and transmission electron microscopy (TEM). The results indicate that the CMMs have a three-dimensional (3D) worm-like mesoporous structure with a surface area between 600 and 800 m(2) g(-1) and the copper ions are incorporated into the matrix with octahedral environment. The catalytic activity of these CMMs in the phenol hydroxylation using H2O2 as oxidant is comparable to that of TS-1. Effects of Cu/Si molar ratio in the catalyst and the influence of various reaction parameters on the catalytic activity were investigated in detail and the optimized reaction condition was acquired. (c) 2006 Elsevier B.V. All rights reserved.