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This work investigated the design and conversion of a research-based comprehensive chemistry experiment in laboratory. The preparation and characterization of carboxylate vanadyl complex is a routine synthetic method in the scientific research on bio-inorganic chemistry. Through the study and optimization all the steps of the experiment which uses the aromatic carboxylic acid to react with the vanadium raw materials, the best experiment conditions, the most efective handling methods and the appropriate reaction time were obtained. The experiment could satisfy the requirements of the stability and reproducibility in teaching experiment. And the carboxylate vanadyl complex products were characterized by the infra-red spectrum (IR) and thermogravimetric analysis (TGA). Through this comprehensive experiment, the students could consolidate the principle of complex preparation, understand and grasp the working principle and operation skiil of the rotary evaporator, microwave oven, infrared spectroscopy and thermogravimetric analyzer, and develop their comprehensive ability including the related chemical basic knowledge, experimental operation, instrument analysis and relevant scientific literacy and research ability. [ABSTRACT FROM AUTHOR]