Zinc　doped　TiO2　mesoporous　hollow　mierospheres　were　synthesized　based　on　sol-gel　method　by　using　SiO2as　the　template,　tetra-n-butyl　titanate　as　Ti　source　and　Zinc　nitrate　hexhydrate　as　Zinc　source.　The　prepared　samples　were　characterized　by　means　of　X-ray　diffraction　(XRD),　low　temperature　nitrogen　adsorption-desorption　(BET　surface　area),　transmission　electron　microscope　(TEM),　scanning　electron　microscopy　(SEM)　and　X-ray　photoelectron　spectroscopy　(XPS).　Methyl　blue　dye　was　used　as　a　target　dye　to　evaluate　the　photocatalytic　activity　of　the　samples.　The　results　show　that　microspheres　are　hollow　after　removing　the　SiO2　template　using　an　aqueous　solution　of　NaOH　and　it　takes　more　than　90　min　to　completely　remove　the　SiO2　template.　The　thickness　of　the　TiO2　shell　is　about　20　nm.　The　dropping　rate　of　tetra-n-butyl　titanate　solution　plays　an　important　role　in　the　structure.　When　the　dropping　time　exceeds　15　min,　the　obtained　hollow　microspheres　have　clear　structure.　The　XRD　results　indicate　that　pure　hollow　microspheres　and　Zinc　doped　hollow　microspheres　exist　in　the　form　of　anatase.　When　the　doping　molar　ratio　of　Zn2+　to　tetra-n-butyl　titanate　is　0.3%,　the　obtained　hollow　microspheres　have　the　smallest　particle　size,　the　biggest　BET　surface　area　and　show　the　most　efficient　degradation　of　methyl　blue　dye.　©　2014,　Chinese　Chemical　Society.All　Rights　Reserved.