In this research, two magnetic nano catalysts of zirconium and palladium, Fe3O4-(3-propyl) trimethoxysilane—natural asphalt sulfonic acid @metal, (metal=Pd and Zr) are synthesized by immobilizing palladium and zirconium nanoparticles on the functionalized natural asphalt sulfonate and, then, characterized using diverse microscopic and spectroscopic techniques. These catalysts are applied as recoverable, efcient and new heterogeneous catalysts for the synthesis of symmetrical and unsymmetrical aryl/alkyl disulfdes by coupling the thiols without using any oxidizing agent. Moreover, the results and behavior of the two catalysts are comparable in some cases. The Fe3O4-PTMS-NAS@M, (M=Pd and Zr), nanocatalysts exhibited efcient magnetization as 38 and 39 emu/g, and are easily separated from the reaction mixture using an external magnet and reused for several runs while maintaining their catalytic activity