Abstract: Aiming at the shortcoming of sodium sulfantimonate preparation process,a new preparation process was designed which adopted sodium sulfide to leach sodium sulfantimonate from sodium antimonate.The new process has many good features,uch as stable ingredients of raw materials,high leaching rate,simple procedure,good quality,no semifinished product,economical and reasonable etc..The influences of such factors as sodium sulfide consumption,leaching temperature and leaching time on leaching rate were investigated in detail.The experimental results showed that the optimum process conditions were：leaching temperature is 95 ℃,leaching time is 3 h,mechanical agitation and weight ratio of sodium sulfide and antimony is 2.8.Under these conditions, the leaching rate can reach 97.42%.In addition，the effect of agitation and retarded-cooling crystallization process on purity of products and the effect of concentration of sodium hydrate on solubility of sodium sulfantimonate were also studied.The prepared products were yellowish crystal with good quality and even particle size.<BR>