In the present study, the sol-gel technique helped to obtain Fe-containing samples with a base of amorphous silicon dioxide from rice husks RH-Fe and RH-Fe-300. These materials are characterized by IR spectroscopy, X-ray phase and X-ray spectral analysis. It was shown that the samples contain silicate structures Si-O-Si(Fe) and are in an amorphous state. Structure of the surface layers of RH-Fe-300 catalyst particles was established for the first time using X-ray photoelectron spectroscopy (XPS) and energy-dispersive spectra (EDX) methods. It was shown that the surface layers of the synthesized particles are oxygen depleted due to oxygen vacancies and silanol groups, therefore defects can form in its structure. Photocatalytic activity of the samples in the phenol oxidation reaction under ultraviolet and solar irradiation in the presence of hydrogen peroxide was studied. It was shown that the degree of phenol decomposition in the presence of RH-Fe for 24 hours under solar irradiation was 92%, in the presence of RH-Fe – 17%. Under two-stage irradiation (ultraviolet and solar), the percentage of phenol decomposition using both catalysts after a day amounted to more than 80%. It was established that RH-Fe-300 catalyst increases oxidation of phenolic compounds in alkaline rice husk hydrolysates under solar irradiation in the presence of hydrogen peroxide.