Аннотация:Silica fillers have been a cornerstone in chemical technology due to their versatility,availability, and ease of integration into various formulations. Recent advancements,including chlorine-free synthesis of alkoxysilanes, have paved the way for alternative materialslike polymethylsilsesquioxane (PMSSO). This study explores the structural evolutionand properties of a hydrophobic PMSSO xerogel, synthesized through hydrolytic polycondensationof methyltriethoxysilane (MTEOS). PMSSO exhibits exceptional hydrophobicity,high specific surface area, and compatibility with polymer matrices, making it a promisingfiller for applications in rubber products, lubricants, and cosmetics. We developed astraightforward synthesis method for producing PMSSO xerogel that avoids toxic solventsand organochlorosilanes, ensuring safety and sustainability. The reaction conditions, particularlythe amount of alkali and neutralization parameters, were found to significantlyinfluence the properties of the final xerogels, such as specific surface area. Optimizationof the synthesis parameters allow for obtaining PMSSO xerogels with a specific surfacearea about 600 m2/g. These findings underscore PMSSO’s potential as a versatile, ecofriendlyalternative to conventional silica fillers, offering tailored properties for diverseindustrial applications.