Activities and structures of metal oxide catalysts signifi cantly rely on the synthesis procedures and conditions. In this study,

a novel solvent-free mechanochemical method was employed to prepare catalysts for the ammoxidation of propylene. Multicomponent

oxide catalysts containing bismuth, iron, cobalt, and molybdenum were successfully synthesized using a ball

mill mixer and zirconia jars without the use of nitric acid. The mechanochemically synthesized catalysts exhibited higher

catalytic performance than traditional catalysts prepared by coprecipitation (CP) and rotary evaporation (RE) methods in

propylene ammoxidation. The synergistic eff ect of the mechanochemical method was investigated using various analyses,

such as inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray diff raction (XRD), scanning electron

microscopy, energy-dispersive X-ray spectroscopy (EDS), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS).

ICP-AES analysis revealed that the ball-mill-based catalysts contained metal elements in designated amounts more accurately

than those prepared by the CP or RE methods. Propylene ammoxidation reactions with ball-milled catalysts showed a

synergistic eff ect and improved acrylonitrile yield, especially at a 50:50 wt% ratio of Bi 2 Mo 3 O 12 to Fe 0.36 Co 0.64 MoO 4 . Comprehensive

analyses, including XRD, SEM–EDS, Raman spectroscopy, and XPS, support the conclusion that the improved

performance of the mechanochemically synthesized catalysts can be attributed to the increased interaction between diff erent

phases prepared under mechanical forces, leading to a favorable change in the oxidation state of iron.