Titanium-modified MCM-41 type mesoporous silica materials were prepared by hydrothermal [Ti-MCM-41(HT)], sol-gel [Ti-MCM-41(SG)] and post-synthesis impregnation [TiO2/MCM-41] methods. The materials were characterized and tested as photocatalysts in the oxidative degradation reaction of 2,4,6-trichlorophenol (2,4,6-TCP) in water. The catalysts showed high initial activity. The produced acetate and chloride ions were found to inhibit the degradation reaction. The Ti-MCM-41(HT) sample showed higher overall activity than the Ti-MCM-41(SG) catalyst. One of the probable reasons for this is the difference in the distribution of the active sites that determines the rates of electron (e(-))-hole (h(+)) recombination within the photoactive species. The HT preparation was found to contain silica-bound titania in higher dispersion, while the SG preparation contained also polymerized species with Ti-O-Ti bonds.