Herein,　TiO2　was　prepared　by　the　hydrolysis　method　in　critic　acid　(with　both　carboxyl　and　hydroxyl　groups)　solution　firstly.　And　then,　the　as-prepared　TiO2　was　calcined　at　50,　150,　250,　350,　and　450　degrees　C,　respectively,　in　order　to　investigate　the　effects　of　the　calcination　temperature　on　the　physicochemical　property　and　the　adsorption　performance　of　TiO2.　The　adsorption　performance　of　the　prepared　TiO2　samples　for　cationic　dye-Methylene　Blue　(MB)　was　also　studied.　The　results　indicated　that　high　calcination　temperature　can　destroy　the　organic　moieties　on　the　TiO2　samples　and　further　influence　the　adsorption　performance　of　TiO2　for　the　removal　of　cationic　dye-MB.