Wet gel and dried xerogel of precipitated tin oxy-hydroxide were subjected to mechanochemical and microwave treatments (MChT and MWT, respectively). The prepared samples were studied using DTA-TG, XRD, FTIR, nitrogen adsorption–desorption. MChT and MWT cause improvement of crystal structure, removal of structural OH-groups and increase mesopores diameter as well as form the meso-macroporous structure. As a result, drastic increase of uranyl-ions sorption for all modified samples is observed. Sorption centers can be divided into three groups: selective cation-exchange, non-selective cation-exchange and anion-exchange.