以高砷精炼铋烟尘为原料，采用盐酸浸出、锑粉还原、水解、盐酸溶解、除杂、水解工艺制备高纯氯氧化锑。盐酸浸出高砷精炼铋烟尘，当盐酸溶液与精炼铋烟尘液固比为3：1、反应时间为4 h、反应温度为80℃、盐酸用量为1.2倍理论用量时，Sb，As，Bi和Pb浸出率分别为99.50％，92.79％，95.12％和85.34％；在盐酸浸出液中加入锑粉还原后水解，当水解温度为20℃、水解时间为1 h、稀释比为10：1时，Sb3+水解率达到98.25％；水解产物经盐酸溶解后加入除杂剂，反应1 h后进行二次水解，经过滤、洗涤、烘干所得产品；产品中Sb质量分数达到75.71％，而杂质As，Pb和Bi的质量分数分别为0.081 9％，0.039 2％和0.118 7％。产品为粒度均匀的菱形颗粒，其化学式为SB4O5Cl2。%Preparation of high-purity antimony oxychloride from high-arsenic refined bismuth dust in a process of hydrochloric acid leaching, antimony powder reduction, hydrolysis, hydrochloric acid dissolution, impurity removal, hydrolysis was studied. In the process of leaching with hydrochloric acid, the leaching rates of Sb, As, Bi and Pb are 99.50%, 92.79%, 95.12% and 85.34% when the ratio of hydrochloric acid solutions to refined bismuth dust is 3:1, reaction time is 4 h, reaction temperature is 80 V, the content of hydrochloric acid is 1.2 times of its theoretical content. Sb5+ is reduced to Sb3+by adding antimony powder into the hydrochloric acid leaching solution, which is then hydrolyzed. The hydrolysis rate of Sb3+ arrives at 98.25% when the reaction temperature is 20 ℃, reaction time is 1 h, and the ratio of water to SbCl3 solution is 10:1. After the hydrolysate is dissolved by hydrochloric acid solutions and the impurity is removed after 1 h by means of adding agent, the solution is hydrolyzed and the products is obtained by means of filtration, washing and drying. The content of Sb in the products arrives at 75.71% and the impurity contents of As, Pb, Bi are 0.081 9%, 0.039 2% and 0.118 7%, respectively. The product is rhombohedral particles with the advantages of uniform size and its chemical formula is Sb4O5Cl2.
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