Thermally stable Al- and Zr-PILC loaded with copper and cobalt cations and silver nanoparticles were synthesized. The structural and surface features of these nanosystems were studied and compared with those of bulk analogs – partially stabilized ZrO2 loaded with the same active components. Specificity of the catalytic properties of nanocomposites in SCR of NO x by propane, propylene and decane in the excess of oxygen appears to be determined both by distribution of active components on the catalytic surface and degree of their interaction with supports. Formation of ads.-NO x , nitroxyl-hydrocarbon C x H y NO2 ⋅ and isocyanate NCO intermediates was observed by ESR and IR spectroscopy in situ.