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钒渣亚熔盐提钒生产过程中钒铬硅分析方法研究

章伟 王宝华 刘超 刘丽颖 吕慧 朱建岩

章伟, 王宝华, 刘超, 刘丽颖, 吕慧, 朱建岩. 钒渣亚熔盐提钒生产过程中钒铬硅分析方法研究[J]. 钢铁钒钛, 2021, 42(5): 92-98. doi: 10.7513/j.issn.1004-7638.2021.05.015
引用本文: 章伟, 王宝华, 刘超, 刘丽颖, 吕慧, 朱建岩. 钒渣亚熔盐提钒生产过程中钒铬硅分析方法研究[J]. 钢铁钒钛, 2021, 42(5): 92-98. doi: 10.7513/j.issn.1004-7638.2021.05.015
Zhang Wei, Wang Baohua, Liu Chao, Liu Liying, Lv Hui, Zhu Jianyan. Study on analytical method of V, Cr and Si in the process of extracting V from vanadium slag by sub-molten salt[J]. IRON STEEL VANADIUM TITANIUM, 2021, 42(5): 92-98. doi: 10.7513/j.issn.1004-7638.2021.05.015
Citation: Zhang Wei, Wang Baohua, Liu Chao, Liu Liying, Lv Hui, Zhu Jianyan. Study on analytical method of V, Cr and Si in the process of extracting V from vanadium slag by sub-molten salt[J]. IRON STEEL VANADIUM TITANIUM, 2021, 42(5): 92-98. doi: 10.7513/j.issn.1004-7638.2021.05.015

钒渣亚熔盐提钒生产过程中钒铬硅分析方法研究

doi: 10.7513/j.issn.1004-7638.2021.05.015
基金项目: 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)。
详细信息
    作者简介:

    章伟(1969—),男,河北承德人,大学,高级工程师,主要从事冶金分析与试验工作。E-mail:18932879108@163.com。

  • 中图分类号: TF841.3

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

  • 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。
  • 图  1  钒铬干扰试验

    Figure  1.  Vanadium chromium interference test

    表  1  钒铬共存试验结果

    Table  1.   Coexistence test results of vanadium and chromium

    样品加入钒量/mg加入铬量/mg测得钒量/mg测得铬量/mg
    1050.00050.00
    250.00049.980
    310.0010.009.9010.11
    425.0025.0025.0424.90
    550.0050.0050.0850.13
    下载: 导出CSV

    表  2  钒渣和尾渣精密度试验结果

    Table  2.   Precision test results of vanadium slag and tailings

    样品
    方法成分
    w/%相对标准偏差
    RSD /%
    测定值平均值
    钒渣化学法V10.69,10.71,10.66,10.75,10.68,10.65,10.72,10.6110.680.41
    Cr1.55,1.56,1.51,1.54,1.54,1.56,1.51,1.491.531.70
    尾渣化学法全V1.05,0.98,1.01,0.99,0.98,1.04,1.04,0.991.012.90
    全Cr0.64,0.62,0.66,0.62,0.64,0.63,0.62,0.630.632.20
    可溶V0.13,0.14,0.13,0.12,0.14,0.12,0.14,0.110.138.66
    可溶Cr0.051,0.048,0.051,0.052,0.052,0.053,0.055,0.0560.0524.79
    下载: 导出CSV

    表  3  结晶溶液精密度试验结果

    Table  3.   Precision test results of crystalline solution

    样品
    方法
    成分
    测定值
    /(g·L−1
    平均值
    /(g·L−1
    相对标准偏差
    RSD/%
    结晶溶液1#化学法V25.45,25.36,25.49,25.28,25.41,5.38,25.34,25.2925.380.29
    Cr43.25,43.46,43.58,43.31,43.45,43.39,43.28,43.3943.390.25
    Si1.36,1.46,1.40,1.42,1.32,1.39,1.40,1.381.392.90
    结晶溶液2#化学法V16.48,16.29,16.33,16.29,16.36,16.28,16.39,16.5416.370.58
    Cr23.54,23.78,23.68,23.46,23.54,23.67,23.58,23.6423.610.43
    Si0.59,0.58,0.59,0.57,0.58,0.59,0.59,0.590.591.29
    下载: 导出CSV

    表  4  钒渣和尾渣加标回收试验结果

    Table  4.   Recovery test results of vanadium slag and tailings

    样品方法成分本底值/%加入量/%测定总值 /%回收率/%
    钒渣化学法V10.661.0011.95102.49
    Cr0.961.001.99101.53
    尾渣化学法全V1.011.001.9898.51
    全Cr0.631.001.6599.82
    可溶V0.131.001.15101.76
    可溶Cr0.0521.001.065101.23
    下载: 导出CSV

    表  5  结晶溶液加标回收试验结果

    Table  5.   Recovery test results of crystalline solution

    样品
    方法
    成分
    本底值
    /(g·L−1
    加入量
    /(g·L−1
    测定总值
    /(g·L−1
    回收率
    /%
    结晶溶液1# 化学法 V 25.38 1.00 26.59 100.79
    Cr 43.39 1.00 44.30 99.80
    Si 1.39 0.50 1.866 98.73
    结晶溶液2# 化学法 V 16.37 1.00 17.57 101.15
    Cr 23.61 1.00 24.49 99.51
    Si 0.59 0.50 1.073 98.44
    下载: 导出CSV
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  • 收稿日期:  2021-07-26
  • 刊出日期:  2021-10-30

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