Abstract:A novel Salphen covalent organic frameworks (Salphen-COF) based on o-phenylenediamine and 1,3,5-triformylphloroglucinol were successfully synthesized by a total green room-temperature solid-state mechanochemical grinding route. FT-IR and XRD spectra show that the solid-state mechanochemically synthesized Salphen-COF has moderate crystallinity with remarkable stability in water, acid and base. Exfoliation of Salphen-COF layers was observed during mechanochemical synthesis by SEM and TEM. After complexing of various metals (including Zn,Ni,Co, Mn) by mechanochemical grinding, M-Salphen can be an effective, green catalyst for the cycloaddition of carbon dioxide to terminal epoxides to afford cyclic carbonates, and Zn(Salphen) has the highest catalytic efficiency.