The　BiOCOOH　with　multi-layered　structure　was　synthesized　by　hydrothermal　method,　and　then　was　used　as　sacrificial　precursor　to　prepare　several　different　products　through　adjusting　heat　treatment　temperatures,　including　a　new　type　of　composite　photocatalytic　material　β-Bi2O3/BiOCOOH　with　visible　light　response.　The　crystal　structure,　optical　absorption　performance,　morphology,　photocurrent　and　other　physical　and　chemical　properties　of　the　products　were　characterized　by　means　of　X-ray　diffraction　(XRD),　UV-Vis　DRS,　scanning　electron　microscope　(SEM),　photoelectric　chemical　response　and　other　characterization　methods.　Their　photocatalytic　activity　was　assessed　via　degradation　test　of　Rhodamine　B　solution.　The　results　show　that　when　the　heat　treatment　temperature　gradually　increased　from　250℃　to　330℃,　400℃　and　450℃,　the　following　transformation　occurred:　BiOCOOH→β-Bi2O3/BiOCOOH→β-Bi2O3→α-Bi2O3.　The　visible　light　catalytic　performance　of　the　composite　photocatalyst　β-Bi2O3/BiOCOOH　is　the　best.　The　degradation　rate　of　Rhodamine　B　in　the　presence　of　β-Bi2O3/BiOCOOH　composite　photocatalyst　was　6.7　times　and　100　times　higher　than　those　in　the　presence　of　β-Bi2O3　and　α-Bi2O3,　respectively.　The　samples　that　showed　the　best　decolorization　rate　for　rhodamine　B　had　a　mineralization　rate　of　88%　within　90　minutes　of　illumination.　Electrochemical　test　results　show　that　the　composite　β-Bi2O3/BiOCOOH　has　a　larger　photocurrent　response　and　a　smaller　impedance　than　the　plain　materials　β-Bi2O3　and　BiOCOOH.　In　addition,　by　considering　both　of　UV-Vis　DRS　and　Mott-Shottky　curves　comprehensively,　the　positions　of　conduction　and　valence　bands　of　β-Bi2O3　and　BiOCOOH　can　be　estimated　respectively,　and　it　is　speculated　that　β-Bi2O3　and　BiOCOOH　can　be　closely　combined　to　form　z-type　photocatalytic　structure,　thus　having　higher　separation　efficiency　of　photogenerated　carriers　and　effective　separation　of　photogenerated　charges.　©　All　right　reserved.