High purity tantalum ethoxide (99.997%) was successfully synthesized using electrosynthesis method and characterized by IR and 1 H-NMR spectra, the influence of various factors on the electrosynthesis process and the distillation purification of tantalum ethoxide was also studied. Cell voltage was closely related to process parameters such as electrolyte species, electrolyte concentration, electrode distance, solution temperature, current density and electrolysis time et al. All the current efficiencies were higher than 100%, which might be related to the low valence sate of tantalum. The ideal conditions for the electrosynthesis of tantalum ethoxide were also obtained. The purity of tantalum ethoxide increased when increasing reflux ratio. Infrared spectra conformed to chemical bonds excellently, and the peak area ratio of nuclear magnetic resonance coincided with number ratio of hydrogen atoms.