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›› 2007, Vol. 7 ›› Issue (1): 75-78.

• 反应与分离 • 上一篇    下一篇

加碳氯化-氧化反应方法从氟碳铈矿-独居石混合精矿中提取稀土

张丽清,张凤春,姚淑华,姜琳琳,王小欢   

  1. 沈阳化工学院应用化学学院
  • 出版日期:2007-02-20 发布日期:2007-02-20

Rare Earth Extraction from Mixed Bastnaesite-Monazite Concentrate by Carbochlorination-Oxidation

ZHANG Li-qing,ZHANG Feng-chun,YAO Shu-hua,JING Lin-lin,WANG Xiao-huan   

  1. Applied Chemistry College Shenyang Institute of Chemical Technology
  • Online:2007-02-20 Published:2007-02-20

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摘要： 以活性炭为还原剂、氯气为氯化剂、SiCl4为除氟剂、O2和H2O混合气体为氧化剂，采用氯化-氧化反应方法从氟碳铈-独居石混合精矿中提取稀土元素. 在脱氟剂SiCl4作用下，随着反应温度由500℃增至800℃，氟碳铈-独居石混合精矿稀土氯化率由92%增至99%，而无SiCl4时同样温度范围内，稀土氯化率为56%~88%，500℃氯化反应2 h时主要产物为稀土氯化物、氯化钙；当氯化反应温度小于500℃时，与原料比钍的氯化产物挥发量小于1.0%. 水洗氟碳铈-独居石混合精矿的焙砂，过滤并在空气中固化得到氯化产物，在550℃, O2+H2O气氛下氧化反应90 min，实现稀土元素和非稀土元素、铈和非铈稀土元素的分离.

关键词: 氟碳铈矿-独居石混合精矿, 脱氟剂, 加碳氯化, 氧化

Abstract: A stepwise carbochlorination-oxidation process was developed for the rare earth extraction from mixed bastnaesite-monazite concentrate using carbon as reductant, chlorine gas as chlorination agent, SiCl4 gas as defluorination agent, and O2+H2O mixed gas as oxidant. Under the temperatures from 500℃ to 800℃, the rare earth chlorinated conversion rate for 2 h was 56% to 88% in the absence of SiCl4, but 92% to 99% in the presence of SiCl4. The residue of carbochlorination of the mixed concentrate at 500℃ for 2 h mainly contained LnCl3 and CaCl2. When the temperature of carbochlorination was below 500℃, the portion of evaporated thorium to the thorium in the raw material was less 1.0%. The product of carbochlorination was leached with water and solidified in air. The subsequent oxidation of the solid chloride mixture in the wet air at 550℃ for 90 min may result in the separation of rare earth elements and non-rare earth elements, and the separation of Ce and non-Ce elements.

Key words: mixed bastnaesite-monazite concentrate, defluorination agent, carbochlorination, oxidation