Abstract: Vanadyl oxalate with high quality was prepared using vanadium pentoxide and oxalic acid as raw materials,and the effects of reaction temperature and time,and adding coefficient of oxalic acid on the quality of vanadyl oxalate solution and reaction process were investigated.The results show that vanadyl oxalate solution satisfying the technical targets can be obtained under the following conditions:2:1 of mass ratio for oxalic acid to vanadium pentoxide and 50~60℃ of reaction temperature.The vanadyl oxalate solid was characterized by XRD,SEM and EDS.It is indicated that the XRD pattern fits well with that of VOC₂O₄·5H₂O,and vanadyl oxalate with high quality can be prepared when the content of Na for raw materials is less than 0.01%.