从铜阳极泥分锑渣中碱浸制备锑酸钠工艺研究

发布时间：2018-08-09 06:59

【摘要】：针对冶炼系统产出的各种含锑废弃料得不到有效回收利用,同时对环境造成污染的现状,在对铜阳极泥分锑渣物性分析的基础上,提出“硫化钠碱浸—氧化沉锑—精制除杂”锑酸钠生产新工艺,为锑资源的回收再利用开辟了新的途径和实际生产工艺提供有意义的参考。本课题针对锑渣硫化钠碱浸和空气催化氧化硫代亚锑酸钠制备锑酸钠过程及其动力学进行研究,得出以下结论:(1)对锑渣采用Na2S+Na OH碱性浸出试验,考察了多种因素对浸锑过程的影响,确定了浸出最佳条件为:硫化钠浓度165 g·L-1,氢氧化钠浓度30-40 g·L-1,固液比1:5,浸出温度85℃-90℃,反应时间1h-1.5h。按上述条件试验,锑浸出率95%,浸出渣含锑6%。Pb、Cu、Ag、Fe等金属入渣率97%,实现了锑与其他金属的分离及杂质金属元素有效的富集。(2)对锑渣的碱浸过程动力学研究发现,在55℃-85℃温度范围内,浸出过程属于化学反应控制,温度对浸出率有显著影响,反应表观活化能为47.86 k J·mol-1。(3)通过对浸出液采用空气催化氧化制备粗锑酸钠实验研究,确定了最佳锑氧化条件为:高锰酸钾加入量0.75 g·L-1,邻苯二酚加入量不超过0.5 g·L-1,鼓风强度1.415m3·m-2·min-1,氢氧化钠过量系数1.5-1.6,反应温度75℃-85℃,氧化时间6 h-8 h。锑的氧化率达到98.06%以上,沉锑后液中锑浓度低于0.3 g·L-1。(4)在氧化硫代亚锑酸钠动力学研究过程中,联合运用孤立法及半衰期法处理实验结果,求出该反应动力学方程式及其表观活化能。在催化条件下该反应动力学方程式:1.1610.4889Sb]×k=[Na OH][ ×dtd[Sb]-反应表观活化能为5.04 k J·mol-1,确定氧化反应控制步骤是扩散传质控制。(5)粗锑酸钠通过酸溶除杂精制,获得具有杂质含量低、白度高优质锑酸钠产品。SEM分析表明,锑酸钠颗粒分布均匀,分散性好,颗粒尺寸大,平均粒度达到80μm。锑总回收率为91.23%。
[Abstract]:In view of the fact that various antimony waste materials produced by smelting system can not be effectively recycled and polluted to the environment, based on the analysis of the properties of antimony separation slag from copper anode slime, A new process for the production of sodium antimony by alkali leaching, oxidation precipitation, purification and removal of impurities by sodium sulfide is proposed, which provides a valuable reference for the recovery and reuse of antimony resources. The preparation and kinetics of sodium antimonate from antimony residue by alkaline leaching of sodium sulphide and air catalyzed oxidation of sodium antimonite were studied in this paper. The following conclusions were obtained: (1) the alkaline leaching experiment of antimony residue with Na2S NaOH was carried out. The effects of various factors on antimony leaching were investigated. The optimum leaching conditions were determined as follows: concentration of sodium sulfide 165 g L -1, concentration of sodium hydroxide 30-40 g L -1, ratio of solid to liquid 1: 5, leaching temperature 85 鈩，

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