Results are presented of the study of sorption of anion-active dye and dichromate ions from aqueous solutions by powders of 35 mol % Al2O3–65%[ZrO2–3% Yb2O3] synthesized by the sol–gel method at 10°C in the presence of polyvinylpyrrolidone are presented. The obtained hydrogels were dried in the traditional way at 180°C and with microwave drying without calcination and with calcination at 500°C. The sorbents were characterized by TG/DSC, XRD, IR spectroscopy, and BET/BJH and tested under conditions of long-term and dynamic sorption. The calcined sample with microwave drying showed there to be an increased degree of extraction of test molecules and surface activity—the initial rate and limiting adsorption calculated from the model of the two-point form of substance adsorption.