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The immobilization of molybdenum (Mo) compounds on poly(4‐vinylpyridine) (P4VP) microspheres for catalytic epoxidation was reported. P4VP‐supported Mo compounds were highly efficient and selective for the epoxidation of cis‐cyclooctene using hydrogen peroxide (H2O2) as oxygen source. When ethanol was used as solvents, outstanding catalytic activity and selectivity were observed for Mo‐containing catalysts in the epoxidation of cis‐cyclooctene. A completely green epoxidation system based on H2O2 and cleaner solvent has been achieved, and the heterogenized Mo catalyst can be recovered for five times without loss of its activity. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 558–562, 2010

Poly 4-vinylpyridine (P4VP) microspheres between 170 and 728 nm were synthesized by Emulsifier-Free Emulsion Polymerization. The monomer concentration, ionic strength, and initiator concentration affected the microsphere size and size distribution. The increasing monomer concentration led to the increase of microsphere size, whereas the size distribution of the resultant P4VP microspheres increased with the increasing ionic strength of the reaction systems. Mo(O 2 ) 2 OÁ2DMF was successfully anchored onto the P4VP microspheres by ligand exchange, and the heterogeneous catalyst showed high-catalytic activity for epoxidation of cis-cyclooctene with environmentally friendly hydrogen peroxide. The size and morphology of the supported microspheres has important influence on the catalytic activity.