钒渣亚熔盐提钒生产过程中钒铬硅分析方法研究  

Study on analytical method of V,Cr and Si in the process of extracting V from vanadium slag by sub-molten salt

作　　者：章伟 王宝华 刘超 刘丽颖 吕慧 朱建岩 Zhang Wei;Wang Baohua;Liu Chao;Liu Liying;Lv Hui;Zhu Jianyan(Chengde Vanadium and Titanium New Material Co.,Ltd.,HBIS Group Co.,Ltd.,Chengde 067102,Hebei,China;HBIS Group Chengsteel Company,Chengde 067102,Hebei,China)

机构地区：[1]河钢承德钒钛新材料有限公司,河北承德067102 [2]河钢集团承钢公司,河北承德067102

出　　处：《钢铁钒钛》2021年第5期92-98,共7页Iron Steel Vanadium Titanium

基　　金：国家2017年绿色制造系统集成项目(钒的清洁提取与产品绿色制造产业化示范,19044011Z)。

摘　　要：研究钒渣亚熔盐提钒生产过程中钒铬硅分析方法。采用过硫酸铵氧化-硫酸亚铁铵滴定法联合测定钒铬含量:在15%~20%的硫酸酸度下,过硫酸铵氧化钒为五价,同时六价铬被还原为三价,消除铬干扰,以此测定钒量;在4%~6%的硫酸酸度下,加入银盐、过硫酸铵,同时氧化钒铬,以此测定钒铬合量,差减法计算铬量。采用硅钼蓝光度法测定结晶溶液中硅浓度,加入亚硫酸钠还原钒铬,消除钒铬干扰;以酚酞为指示剂,加入硫酸,调节硅钼黄生成时酸度为0.3 mol/L;选择波长660 nm处测量显色液吸光度,绘制工作曲线,计算硅浓度。同时进行方法精密度和加标回收试验,结果令人满意。The analysis method of vanadium,chromium and silicon in the process of vanadium extraction from vanadium slag by sub-molten salt was studied.The content of vanadium and chromium was determined by ammonium persulfate oxidation and ammonium ferrous sulfate titration.At 15%~20%sulfuric acid acidity,ammonium persulfate oxidizes vanadium to a pentavalent state,while Cr(VI)is reduced to Cr(III)to eliminate chromium interference and determine the amount of vanadium.In 4%~6%sulfuric acid acidity,add silver salt and ammonium persulfate at the same time for oxidization of vanadium and chromium,in order to determine the amount of vanadium and chromium,and the amount of chromium is calculated by difference subtractive method.The concentration of silicon in the crystallization solution was determined by silicon molybdenum blue photometric method.Add sodium sulfite to reduce vanadium and chromium and eliminate the interference of vanadium and chromium.With phenolphthalein as indicator,sulfuric acid was added to adjust the acidity of silicon molybdenum yellow to 0.3 mol/L.The absorbance of the color solution was determined at the wavelength of 660 nm,and the working curve was drawn to calculate the silicon concentration.At the same time,the method precision and standard addition recovery tests were carried out,and the results were satisfactory.

关 键 词：钒渣 亚熔盐提钒 钒 铬 硅 分析方法 

分 类 号：TF841.3[冶金工程—有色金属冶金]