Three　dimensional　(3D)　flower-like　α-FeOOH　nanomaterials　were　prepared　by　oil　bath　reflux　method　using　FeSO4,　urea,　ethanol　and　water,　and　the　products　which　were　characterized　by　XRD,　FT-IR　and　SEM　techniques.　The　SEM　images　showed　that　the　3D　flower-like　samples　consisted　of　nanorods　with　a　length　of　400-500　nm　and　a　diameter　of　40-60　nm.　The　catalytic　performance　of　the　samples　was　evaluated　by　catalytic　degradation　of　diclofenac　sodium　using　H2O2　as　the　oxidant　under　simulated　visible　light.　The　results　showed　that　the　as-prepared　samples　presented　high　efficient　catalytic　performances,　and　more　than　99%　of　the　initial　diclofenac　sodium　(30　mg·L-1)　was　degraded　in　90　min.　A　radical　mechanism　can　be　proposed　for　the　catalytic　degradation　of　diclofenac　sodium　solution.　©,　2015,　Science　Press.　All　right　reserved.