Development of photocatalyst is a key step for separation of photocatalyst to solution supported materials. ZnO-Ag/MCM-41 nanoparticles synthetized by a wet process were studied as photocatalysts in the Congo red photodegradation, which is a water contaminant. Also were used prepared zinc oxide, commercial zinc oxide, silver doped zinc oxide, Mobil Catalytic Material No. 41, zinc oxide supported on MCM-41, and commercial zinc oxide supported on MCM-41. All systems were characterized by SEM, FTIR, XRD, and surface area by BET and tested in photocatalytic degradation of Congo red. It was found that the systems showed the crystalline phase wurtzita for ZnO, and a main amorphous component for MCM-41, ZnO/MCM-41 and ZnOC/MCM-41. The materials had different particle size and morphology; however, predominantly spherical nanoparticles (less than 100 nm) were found. For photocatalytic UV irradiation a maxima degradation of 30% for 120 min was reached with a ZnO-Ag as catalyst.