The zinc oxalate fine particles were prepared by using an emulsion liquid membrane (ELM) system with kerosene as solvent,P204 as extractant (cation carrier),and T155 as surfactant. Zinc ions were extracted from the external phase and stripped into the internal phase to form zinc oxalate particles. The reaction reached equilibrium after 40min and the extraction ratio of zinc ions was 90%. The effects of reaction conditions on the size of particles were investigated. In the range of experiments,the size of particles decreased with increasing surfactant concentration and O/A ratio. The decrease of zinc ions concentration could effectively reduce particle size. Instrumental analysis,such as scanning electron microscopy (SEM),x-ray diffraction (XRD) and thermogravimeter (TG),confirmed that zinc oxalate particles were synthesized. The zinc oxide particles were obtained by calcining zinc oxalate particles at 500℃ for two hours.