Zirconium n-butoxide was successfully synthesized using electrochemical method and characterized by IR and 1 H-NMR spectra. The influence of various factors on the cell voltage of electrosynthesis process was studied. The cell voltage increased with an increase of electrode distance and current density, but decreased with the increasing Bu n 4 NBr concentration and solution temperature. The ideal conditions for electrosynthesis of zirconium n-butoxide were obtained. The resulting zirconium n-butoxide solution was purified by distillation and n-hexane extraction. Infrared spectra conformed to chemical bonds excellently, and the peak area ratio of nuclear magnetic resonance coincided with number ratio of hydrogen atoms in Zr(OC 4 H 9 ) 4 . The purity was close to 99.99%.