高纯三氯化锑的提纯工艺研究

Research on the Purification Process of High Purity Antimony Trichloride

以国标级99.80%三氧化二锑为原料,研究了合成三氯化锑时盐酸比例、蒸发温度、精馏提纯釜内温度等因素对高纯三氯化锑制备的影响。研究结果表明:三氧化二锑合成三氯化锑时,盐酸用量为化学计量比的1.5倍;三氯化锑母液蒸发浓缩工序中,120℃的釜温能够有效提升砷元素的脱除率;精馏提纯工序,控制回流比8∶3,精馏釜温223.8~230℃内精馏分馏出来的SbCl_(3)产品满足后续高纯锑(6N级以上)制备要求,As、Pb、Bi含量都小于0.05 mg/kg。本研究有效扩大了高纯锑生产对三氧化二锑原料的选择范围,对实现批量化高纯锑的生产有着非常重要的意义。

The influence of factors such as hydrochloric acid ratio,evaporation temperature and temperature inside the distillation and purification kettle on the preparation of high-purity antimony trichloride was studied using 99.80%antimony trioxide,a national standard grade raw material.The research results indicated that when synthesizing antimony trichloride from antimony trioxide,the amount of hydrochloric acid used was 1.5 times the stoichiometric ratio,in the evaporation and concentration process of antimony trichloride mother liquor,a kettle temperature of 120℃could effectively improve the removal rate of arsenic elemen,the distillation purification process controled the reflux ratio of 8∶3,and SbCl_(3) product obtained by distillation distillation at a temperature of 223.8~230℃in the distillation kettle met the requirements for the subsequent preparation of high-purity antimony(6N grade or above),with As,Pb and Bi contents all less than 0.05 mg/kg.This study effectively expanded the selection range of antimony trioxide raw materials for high-purity antimony production,which was of great significance for achieving batch production of high-purity antimony.