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    从富硒石煤回收制备粗硒的新工艺

    田欢 帅琴 徐生瑞 鲍征宇 谢淑云

    田欢, 帅琴, 徐生瑞, 鲍征宇, 谢淑云, 2014. 从富硒石煤回收制备粗硒的新工艺. 地球科学, 39(7): 880-888. doi: 10.3799/dqkx.2014.082
    引用本文: 田欢, 帅琴, 徐生瑞, 鲍征宇, 谢淑云, 2014. 从富硒石煤回收制备粗硒的新工艺. 地球科学, 39(7): 880-888. doi: 10.3799/dqkx.2014.082
    Tian Huan, Shuai Qin, Xu Shengrui, Bao Zhengyu, Xie Shuyun, 2014. Novel Technology for Preparation of Crude Selenium from Se-Rich Stone Coal. Earth Science, 39(7): 880-888. doi: 10.3799/dqkx.2014.082
    Citation: Tian Huan, Shuai Qin, Xu Shengrui, Bao Zhengyu, Xie Shuyun, 2014. Novel Technology for Preparation of Crude Selenium from Se-Rich Stone Coal. Earth Science, 39(7): 880-888. doi: 10.3799/dqkx.2014.082

    从富硒石煤回收制备粗硒的新工艺

    doi: 10.3799/dqkx.2014.082
    基金项目: 

    中国地质调查局项目 1212011120324

    中国地质调查局项目 12120113087100

    中国地质调查局项目 12120113087000

    详细信息
      作者简介:

      田欢(1988-), 男, 硕士研究生, 研究方向为环境地球化学.E-mail: tianhuanvip@126.com

      通讯作者:

      鲍征宇, E-mail: zybao@cug.edu.cn

    • 中图分类号: TD983;X752

    Novel Technology for Preparation of Crude Selenium from Se-Rich Stone Coal

    • 摘要: 通过实验研究了湖北恩施富硒石煤燃烧中烟气硒的回收, 提出了一条回收制备粗硒的有效途径, 即采用高效钙基吸附剂固定石煤燃烧排放的硒, 用亚硫酸钠还原硒化合物制备出粗硒产物.模拟实验确定了Na2SO3还原硒的最佳条件: 还原温度353 K, 还原时间15 min, HCl浓度4 mol·L-1, 亚硫酸钠加入量(质量比)Na2SO3∶Se最佳比值为6, 硒的回收率达98.48±1.95%(n=3), 在实验应用中也得到了较好的回收率.XRD和SEM-EDS分析表明产物硒的晶型和纯度等是受反应体系中多种因素共同影响的.

       

    • 图  1  研究区示意(据郭宇等,2012)

      Fig.  1.  Sketch of the study aera

      图  2  实验装置示意

      Fig.  2.  Schematic diagram of experimental apparatus

      图  3  温度对硒还原率的影响

      Fig.  3.  Effect of temperature on reduction rate of selenium

      图  4  时间对硒还原率的影响

      Fig.  4.  Effect of time on reduction rate of selenium

      图  5  盐酸浓度对硒还原率的影响

      Fig.  5.  Effect of HCl concentration on reduction rate of selenium

      图  6  还原剂用量(质量比)对还原的影响

      Fig.  6.  Effect of mass ratio between Na2SO3 and Se on reduction of selenium

      图  7  无定型红色硒单质实物

      Fig.  7.  The object picture of amorphous red elemental selenium

      图  8  模拟实验产物硒单质的XRD谱

      Fig.  8.  XRD spectrum of Se in simulant experiment

      图  9  模拟实验产物硒的SEM图像(a)和EDS谱图(b)

      Fig.  9.  SEM image (a) and EDS spectrogram (b) of elemental Se in simulant experiment

      图  10  恩施石煤燃烧烟气吸附实验中产物硒的SEM图像(a)和EDS谱图(b)

      Fig.  10.  SEM image (a) and EDS spectrogram (b) of amorphous Se in combustion flue gas adsorption of Se-rich stone coal from Enshi

      表  1  富硒石煤工业分析和元素分析

      Table  1.   Industry analysis and Elemental analysis of Se-rich stone coal

      工业分析(%) 元素分析(%)
      成分 水分 灰分 挥发分 固定碳 C H O N S
      恩施石煤 1.61 62.09 8.73 27.57 30.58 2.72 2.05 0.18 0.78
      下载: 导出CSV

      表  2  煤样和煤灰中主要氧化物的XRF分析

      Table  2.   Concentration of major oxides in coal and ash after combustion determined by XRF

      元素 煤样(%) 煤灰(%)
      SiO2 75.78 78.14
      Al2O3 13.45 14.74
      SO3 3.21 0.06
      K2O 2.21 2.11
      V2O5 1.58 1.47
      MgO 1.27 1.33
      Fe2O3 0.82 0.75
      TiO2 0.47 0.43
      Cr2O3 0.43 0.41
      P2O5 0.32 0.31
      MoO3 0.15 0.12
      SeO2 0.14
      CaO 0.09 0.07
      NiO 0.06 0.05
      ZrO2 0.02 0.01
      下载: 导出CSV

      表  3  还原回收实验实际应用效果

      Table  3.   The actual application effect of recovery experiments

      实验 实验1 实验2 实验3 均值 偏差
      回收率(%) 70.94 75.1 72.77 72.94 2.09
      滤液含硒率(%) 12.55 10.78 9.17 10.84 1.69
      注:还原条件:温度353 K;时间15 min;HCL浓度4 mol·L-1;Na2SO3∶Se=6∶1.
      下载: 导出CSV
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