NaxBayBiO3　center　dot　nH(2)O　(NBBO)　has　been　prepared　using　a　commercial　NaBiO3　center　dot　nH(2)O　(NBO)　as　a　starting　material　with　a　hydrothermal　iron-exchange　reaction.　As-synthesized　samples　were　characterized　by　means　of　X-ray　diffraction　(XRD),　scanning　electron　microscopy　(SEM),　ultraviolet-visible　light　(UV-vis)　absorbance　spectra,　thermogravimetry-differential　scanning　calorimetry　(TG-DSC)　and　X-ray　photoelectron　spectroscopy　(XPS)　techniques.　The　photooxidation　decomposition　of　phenol　over　NBBO　has　been　carried　out　under　visible-light　irradiation　(lambda　＞　400　nm).　The　result　revealed　that　the　NBBO　showed　considerable　photooxidation　activity　for　phenol　degradation　in　the　range　of　visible　light.　The　result　of　reusability　indicated　the　structure　of　NBBO　was　instable,　which　was　changed　to　Bi2O2CO3　in　the　photooxidation　process,　although　photooxidation　activity　kept　high　in　three　runs.　This　study　has　provided　useful　information　for　the　development　of　new　bismuthate　photocatalyst　with　higher　photoactivity　under　visible-light　irradiation.　(C)　2009　Elsevier　B.V.　All　rights　reserved.