摘要
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 ℃,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.
出处
《中南大学学报（自然科学版）》
EI
CAS
CSCD
北大核心
2011年第6期1549-1554,共6页
Journal of Central South University:Science and Technology
基金
广东省教育部产学研重大项目(2008A090300016)
关键词
精炼铋烟尘
盐酸浸出
除杂
氯氧化锑
refined bismuth dust
hydrochloric acid leaching
removing impurities
antimony oxychloride
