The technology of obtaining porous nanostructures is based on ecological organosilicon materials and their uses in some spheres of human life, for example, for medical preparations, for thermal insulation of building structures and industrial equipment, and for cleaning. The purpose of this study was to establish correlations between various experimental parameters (shear stress, speed pulsations, temperature, viscosity, and processing time) and the rheological characteristics of suspensions obtained by the method of liquid-phase dispersion; it was a study of hydrodynamic effects and the processes of heat and mass exchange in liquid systems during the liquid-phase dispersion of hydrogel monoliths by means of discrete-pulse activation in a special rotary apparatus. The dehydration of hydrogels was carried out by two methods: convective drying in a layer and spraying in the coolant flow. Experiments have shown that the key parameters for obtaining stable homogeneous suspensions are a synergistic combination of concentration factors and processing time. To obtain adsorbents in the form of pastes with specified adsorption properties and a monolith size of up to 300 μm, the optimal parameters were a hydrogel concentration of 70% and a processing time in the double-recirculation mode. Xerogels obtained by convective drying are a polydisperse mixture of strong monoliths and fragile aggregates. In contrast, xerogel monoliths obtained by spray drying show great homogeneity in terms of dispersion and strength characteristics. The rheological parameters of the hydrogel dispersions, which depend on the concentration and hydrodynamic treatment modes, are the dominant factors affecting the moisture extraction during drying. This study marks the first investigation into the resilience of porous organosilicon structures against the influence of intense turbulence fields and mechanical stresses experienced within the rotor apparatus during suspension production.