The electrochemical preparation of antimony trioxide (Sb2O3) employing an antimony anode and a stainless steel cathode is described. The effects of different electrolytes, electrolyte concentration, pH, temperature, anode current density, different cathode materials, and different additives on current efficiency and purity for the preparation of antimony trioxide were studied. A maximum current efficiency of 99.2% was achieved corresponding to the energy consumption of 1.26 kWh center dot kg(-1).