低浓度失效含铑均相催化剂回收铑的工艺研究

Study on the Process of Recovering Rhodium from Spent Homogeneous Catalyst Containing Low Concentration Rhodium

本研究以乙酸酐生产中使用的失效铑催化剂作为试验原料,采用氧化络合-硫化沉淀工艺高效富集和回收高价值金属铑。研究表明,在氧化络合沉淀试验的最佳工艺中,H_(2)O_(2)用量为40 mL,HCOOH+C_(2)H_(2)O_(4)用量为40 mL,反应温度为70 ℃,络合沉淀时间为120 min,最佳条件下铑回收率达到94.88%;络合沉淀后液硫化沉淀富集铑试验的优化参数中,溶液初始pH为1,反应温度为70 ℃,Na_(2)S用量为10 g,反应时间为150 min,优化条件下铑沉淀率达到70.55%。经过两步工艺处理,铑的综合回收率高达96.39%。

In this study,the spent rhodium catalyst used in acetic anhydride production is used as the test material,and the oxidation complexation-sulfurization precipitation process is used to efficiently enrich and recover high value rhodium metal.The research shows that in the optimal process of oxidation complexation precipitation test,the amount of H_(2)O_(2) is 40 mL,the amount of HCOOH+C_(2)H_(2)O_(4) is 40 mL,the reaction temperature is 70℃.,the complexation precipitation time is 120 min,under the optimal conditions,the rhodium recovery rate reaches 94.88%;in the optimization parameters of rhodium enrichment test by sulfide precipitation of complexed precipitation solution,the initial pH of the solution is 1,the reaction temperature is 70℃,the amount of Na_(2)S is 10 g,and the reaction time is 150 min,under the optimization conditions,the rhodium precipitation rate reaches 70.55%.After two steps of processing,the comprehensive recovery rate of rhodium is 96.39%.