Silicas of highly dispersion degree were obtained. This process includes formation of silica particles and their aggregation. The ethylene glycol solution was used in precipitation process. resulting in a partial blocking of the silica surface hydroxyl groups (silanol groups) and, thus, in a decreased hydrophilicity of silica. Studies on the surface modification of silicas using silane coupling agents are described. The best modifiers were selected, which inducted a change of the silica surface from hydrophilic to hydrophobic. Basic physicochemical analyses of the obtained silicas were performed. The methods of evaluating the degree of surface modification of the silica were presented. Near infrared spectroscopy (NIR) was used to determine the degree of condensation of the silica surface silanol groups. The degree of hydrophobization of silica surface was determined by a calorimetric method. Moreover. studies on morphology and microstructure using transmission electron microscopy (TEM) were performed. Size distribution of primary particles and aggregates and agglomerates structures were determined by ZetaPlus instrument using dynamic light scattering (DLS) method.