This research focuses on the preparation of metal chitosan microspheres using a one-step method,involving the dropping of a chitosan-metal salt mixture into an alkaline solution.These chitosan microspheres contain well-dispersed nanoparticles of MnO2 and Fe3O4(MnO2-Fe3O4/CS)and were used for the Fenton-like degradation of Congo red(CR).Results showed that the catalytic activity of MnO2-Fe3O4/CS was better than that of monometallic chitosan microspheres(MnO2/CS,Fe3O4/CS).Under the optimized conditions(50 mg/L CR,pH=7,0.9 mol/L H2O2,2.0 g/L catalyst,60 min),the removal of CR reached 100%.The improved performance of MnO2-Fe3O4/CS can be attributed to its large specific surface area,high pore volume,and unique porous structure.These characteristics promote the adsorption/diffusion of reactants and the exposure of active site.Moreover,the synergistic effect of Mn and Fe bimetal enhances electron transfer and greatly improves catalytic activity.In addition,the metal chitosan microspheres can be easily collected from the solution and maintain a high activity(88.2%)even five times of reuse.