The controlling sol-gel synthesis of ZrO2 from chlorite or nitrate zirconyl in presence of structures forming polymer agent and introduced silver, copper, gold ions, as active sites for adsorption and catalysis, has been carried out. In direct method (precipitator NH4OH was added to ZrOCl2 aqueous solution) the particles size is greater than in case of reversed method (ZrOCl2 solution was added to NH4OH). The polymer introduction in sol-gel process for both methods leads to decreasing in several times the particles size of hydrated and crystalline ZrO2. Ions additives augmented the surface acidity with increasing activity of pyridine test adsorption in row Ag +