合成硫代锑酸锑的工艺研究

Study on Preparation of Antimony Thioantimonate

研究了用锑酸钠合成硫代锑酸锑的新工艺。新工艺采用硫化钠浸取锑酸钠制取硫代锑酸钠(五价锑),用含盐酸的氯化钠饱和溶液浸取锑白,制取三氯化锑(三价锑)之后,在HCl+NaCl+H2O的反应体系中合成硫代锑酸锑。探索了合成硫代锑酸锑的反应体系,以及pH值、氯化钠浓度、温度、反应时间、洗涤等条件对合成硫代锑酸锑的影响。为避免三价锑水解,设计了HCl+NaCl+H2O的反应体系。制得的产品锑的质量分数为64.1%,S的质量分数为33.8%,接近于硫代锑酸锑的理论含锑、硫总量65.55%、34.45%,达到了较好的产品质量。

The new technique of antimony thioantimonate prepared from sodium pyroantimonate was researched in this paper.The processing technique was as follows:sodium sulfantimonate(pentavalent stibium)was prepared by sodium pyroantimonate leached in sodium sulfide solution,and antimony trioxide was leached with sodium chloride saturated solution and hydrochloric acid,both of which were then added to the reaction system of HCl+NaCl+H2O to synthesize into antimony thioantimonate.The influences of the reaction system of HCl+NaCl+H2O,pH value,concentration of sodium chloride,temperature,time and washing on synthesize of the antimony thioantimonate were researched,and the reaction of HCl+NaCl+H2O was also designed in order to avoid hydrolysis of Sb3+.The production which antimony content was 64.1% and sulphur content was 33.8%,were close to theoretical content of antimony(65.55%)and sulphur content(34.45%).