As an alternative approach for conventional mechanochemical synthesis, a novel gas-solid two-phase flow (GSF) synthetic technique for the mechanochemical synthesis of dual metal-organic frameworks (DMOFs) was reported for the first time. The prepared CoMn 2 (BTC) 2 was characterized by FT-IR, DTA, TG/DTG, and XRD studies. The results indicated that CoMn 2 (BTC) 2 (BTC = 1,3,5-benzenetricarboxylate) was successfully synthesized after 10 min at a rate of 60 kg h -1 . CoMn 2 O 4 microspheres were also prepared via the CoMn 2 (BTC) 2 precursor method and characterized using FT-IR, XPS, XRD, SEM, EDS, and BET methods. The electrochemical properties of the as-prepared CoMn 2 O 4 were investigated, and the GSF results showed that the microsphere electrodes of CoMn 2 O 4 had a high specific capacitance (969 F g -1 ) at a current density of 1 A g -1 in 3 M aqueous KOH solution.