(1. 中南大学 冶金与环境学院，长沙 410083；
2. 有色金属资源循环利用湖南省重点实验室，长沙 410083；
3. 有色金属资源循环利用湖南省工程研究中心，长沙 410083)
摘 要: 针对酸性多金属浸出液中锑分离回收困难的问题，提出采用萃取-反萃水解法，短流程高效率地回收浸出液中的锑，得到锑水解产物。探索了有机相组成、相比O/A、萃取时间、反萃液浓度等因素对萃取及反萃过程的影响。结果表明，最佳工艺条件如下：萃取条件为有机相组成50%TBP+50%磺化煤油(体积分数)、相比O/A 1:1、操作温度25 ℃、萃取时间30 min、震荡频率120 Hz、单级萃取，反萃条件为稀硫酸溶液0.25 mol/L、反萃时间30 min、相比O/A 1:1。在该条件下处理后，浸出液中80.5%的锑富集于锑水解产物中。在600 ℃下对固体产物进行热处理，得到物相为SbO2和Sb2O4的锑氧化物。
关键字: 高酸复杂含锑溶液；溶剂萃取；磷酸三丁酯；锑氧化物
（1. School of Metallurgy and Environment, Central South University, Changsha 410083;
2. Hunan Key Laboratory of Nonferrous Metal Resources Recycling, Changsha 410083;
3. Hunan Engineering Research Center of Nonferrous Metal Resources Recycling, Changsha 410083）
Abstract:In order to solve the problem of antimony recovery in acid multimetallic leachate, the extraction-stripping hydrolysis was proposed to recover the antimony in the leachate, and antimony hydrolysates were obtained efficiently. The effects of organic phase composition, volume ratio between liquor and origanic phase, extraction time and the concentration of stripping solution on extraction and stripping process were explored. The results show that the optimum extraction conditions are as follows: the organic phase consists of 50% TBP+50% sulfonated kerosene (volume fraction), the operating temperature of 25 ℃, O/A of 1:1 the extraction time of 30 min, the oscillation frequency of 120 Hz and single stage extraction. The conditions of dilute sulfuric acid solution is 0.25 mol/L, stripping time is 30 min, O/A is 1:1. After treatment under this condition, 80.5% of the antimony in the leachate is enriched in antimony hydrolysates. The solid product is heat-treated at 600 ℃ to obtain antimony oxide with SbO2 and Sb2O4 phases.
Key words: antimony-bearing complex solution with high acidity; solvent extraction; tributyl phosphate; antimony oxide
