In the study the mechanochemical treatment procedure was used to prepare composite materials based on SiO2 with the addition of TiO2 and carbon black as a carbon matter. The investigations were carried out at the three rotational speeds 300, 500 and 700 rpm. Thermal and structural characteristics of the composites were investigated using N2 adsorption, TG/DTG/DTA, SEM and FT-IR/PAS methods. The photocatalytic properties were evaluated by methylene blue degradation (Co = 1 × 10−5 mol L−1) at UV light. The obtained results show that the mechanochemical treatment at different rotational speeds causes intensive changes in the porous structure of the obtained materials. Thermal analysis proved that the obtained materials are characterized by significant thermal stability. The obtained composites have comparable photocatalytic properties with pure TiO2 despite the fact that in the composite only 5% of TiO2 is used.