陈昆昆,李林波,操齐高,孟晗琪.从沉钨钼后液中制备高纯铼酸铵[J].稀有金属材料与工程,2022,51(8):3049~3056.[Chen Kunkun,Li Linbo,Cao Qigao,Meng Hanqi.Preparation of high purity ammonium rhenate from the solution after precipitation of tungsten and molybdenum[J].Rare Metal Materials and Engineering,2022,51(8):3049~3056.]
从沉钨钼后液中制备高纯铼酸铵
投稿时间:2021-07-21  修订日期:2021-11-01
中文关键词:  沉钨钼后液  铼酸钾  浓缩结晶  离子交换  铼酸铵
基金项目:国家重点研发计划项目(2018YFC1901704)
中文摘要:
      沉钨钼后液首先经氯化钾沉淀反应得到铼酸钾,其次采用离子交换法将铼酸钾溶液转为高铼酸溶液,最后经氨水中和-浓缩结晶-重结晶得到高纯铼酸铵。结果表明:向沉钨钼后液中加入KCl固体再浓缩析出KReO4白色晶体,其主要杂质Na、Ca、Fe、Cl含量均小于1%,特别是W、Mo含量均小于0.1%,且Re结晶率可达94%~98%。采用动态法脱K,选用C160(H+型)树脂,当KReO4溶液pH为中性,料液流速控制为2 BVs.h-1时,C160树脂对K+穿透容量和饱和容量分别为117.865 g.L-1和128.385 g.L-1,且树脂利用率达到91.81%;所得纯HReO4溶液中K、Na、Ca、Fe、W、Mo、Mg浓度均降至0.5 mg.L-1以下。通过添加优级纯氨水中和HReO4溶液,控制终点pH为7~8,再经浓缩结晶+1次重结晶,所得铼酸铵纯度达到99.99%以上,其SEM形貌为树枝状。
Preparation of high purity ammonium rhenate from the solution after precipitation of tungsten and molybdenum
英文关键词:Solution after precipitation of tungsten and molybdenum  potassium rhenate  concentrated crystallization  ion exchange  ammonium rhenate
英文摘要:
      Potassium rhenate was obtained from the solution after precipitation of tungsten and molybdenum by potassium chloride precipitation reaction. Then potassium rhenate solution was converted into perrhenic acid solution by ion exchange method. Finally, high purity ammonium rhenate was obtained by ammonia neutralization - concentrated crystallization - recrystallization. The results show that KCl solid is added to the solution after precipitation of W and Mo, and then concentrated to precipitate KReO4 white crystal. The contents of main impurities Na, Ca, Fe and Cl in potassium rhenate are less than 1%, especially W and Mo are less than 0.1%, and the crystallization rate of Re can reach 94% ~ 98%. K is removed by dynamic method with C160 (H+ type) resin. When the pH of KReO4 solution is neutral and the flow rate of feed is 2 BVs.h-, the K + penetration capacity and saturation capacity of C160 resin are 117.865 g.L-1 and 128.385 g.L-1, respectively, and the utilization rate of resin reaches 91.81%. The concentrations of K, Na, Ca, Fe, W, Mo and Mg in the obtained pure HReO4 solution are all below 0.5 mg.L-1. The HReO4 solution is neutralized by adding high - grade pure ammonia, controlling the end-point pH to 7 ~ 8, and then concentrated and crystallized with one recrystallization. The purity of the obtained ammonium rhenate is more than 99.99%, of which the SEM morphology is dendritic.
作者单位E-mail
陈昆昆 西安建筑科技大学 冶金工程学院 chenk_007@163.com 
李林波 西安建筑科技大学 冶金工程学院  
操齐高 西北有色金属研究院  
孟晗琪 西北有色金属研究院  
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