真空挥发法脱除钼硫化后液中负二价硫的研究  

Removal of negative divalent sulfur in the sulfidation solution of molybdate by vacuum volatilization

作　　者：董宏伟 曹才放 徐志峰 王刚 何志聪 张柏朝 DONG Hongwei;CAO Caifang;XU Zhifeng;WANG Gang;HE Zhicong;ZHANG Baichao(School of Metallurgical and Chemical Engineering,Jiangxi University of Science and Technology,Ganzhou 341000,China)

机构地区：[1]江西理工大学冶金与化学工程学院,江西赣州341000

出　　处：《有色金属科学与工程》2018年第4期9-13,28,共6页Nonferrous Metals Science and Engineering

基　　金：国家自然科学基金资助项目(51404113);江西省教育厅青年科学基金资助项目(GJJ14453)

摘　　要：采用真空挥发的方式将钼硫化后液中的游离负二价硫脱除.考察了铵硫比、挥发时间、温度、钨钼浓度等因素对硫挥发以及后续季铵盐萃取除钼的影响.结果表明,挥发温度和铵硫比是影响硫挥发率的重要因素.在真空度-80 kPa、挥发温度60℃、铵硫物质的量比大于3,可获得较优的硫挥发率;真空挥发过程中,铵分解产生的氢离子可促进钼的硫化反应,有利于钨钼分离.含钼溶液充分硫化反应后,采用真空挥发的操作,既可回收部分硫,还可在后续季铵盐萃取过程中获得更好的除钼效果;当溶液中铵浓度过高,真空挥发进行到一定程度时则会使部分钨结晶析出.The vacuum volatilization method was used to remove the free negative divalent sulfur in the sulfidation solution of molybdate. The effects of ammonium-sulfur ratio, volatilization time, temperature,tungsten and molybdenum concentration on the sulfur volatilization and the molybdenum removal during the subsequent quaternary ammonium salt extraction were investigated. The results show that the volatilization temperature and ammonium-sulfur ratio are important factors affecting the sulfur volatilization rate. Under the condition of-80 kPa, volatilization temperature 60 ℃ and ammonium-sulfur mole ratio greater than 3, a better sulfur volatilization rate can be obtained. Furthermore, the hydrogen ions produced by ammonium decomposition in the process of vacuum volatilization facilitate the sulfidation reaction of molybdate, which is beneficial to the separation of tungsten and molybdenum. After fully sulfidation of molybdate solution, the vacuum volatilization operation can not only recover some sulfur, but also obtain better molybdenum removal effect in the subsequent quaternary ammonium salt extraction process. However, some tungsten-containing crystals will be formed when the ammonium concentration in the solution is too high and the vacuum volatilization is carried out to a certain extent.

关 键 词：除钼 硫化反应 硫化氢 真空挥发 溶剂萃取 

分 类 号：TF111.3[冶金工程—冶金物理化学]