Electrolysis of solid MoS2 in molten CaCl2 for Mo extraction without CO2 emission
Electrolysis of solid MoS2 in molten CaCl2 for Mo extraction without CO2 emission
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DOI：
10.1016/j.elecom.2007.05.007
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发表时间：
2007-08
影响因子：
5.4
通讯作者：
Guoming Li;Dihua Wang;Xianbo Jin;G. Chen
中科院分区：
文献类型：
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作者：
Guoming Li;Dihua Wang;Xianbo Jin;G. Chen
烧结（300°C）的MoS 2多孔颗粒在氩气下在1.0-3.0V下在熔融CaCl 2（800-900°C）中电解1- 20小时以得到元素S和Mo。在石墨阳极上，产物主要是S（但这项工作还不能排除痕量的CS2），并从熔融盐中蒸发，使电解继续进行。然后，它在系统的较低温度区域冷凝成固体。阳极在重复使用后保持完整。MoS_2球团在高温下具有高导电性，可快速电还原成0.1-1.0μm的Mo粉，其中S含量可低于1000 ppm。在低于0.5V的电压下没有发生降低。在0.5-0.7V电压范围内，MoS 2发生部分还原，转化为MoS 2和Mo 3S 4或Mo 3S 4和Mo的混合物，Mo含量随电压的升高而增加。MoS 2粉末在Mo-腔电极中的循环伏安法以及电解结果表明，还原机理包括两个步骤：MoS 2在-0.28V（potential vs. Ag/AgCl）下还原为Mo 3S 4，然后在-0.43V下还原为Mo。
Sintered (300°C) porous pellets of MoS2were electrolysed to elemental S and Mo in molten CaCl2(800–900°C) under argon at 1.0–3.0V for 1–20h. On a graphite anode, the product was primarily S (but traces of CS2could not yet be excluded by this work) and evaporated from the molten salt, allowing the electrolysis to continue. It then condensed to solid at the lower temperature regions of the system. The anode remained intact after repeated uses. The MoS2pellet was highly conducting at high temperatures and could be fast electro-reduced to fine Mo powders (0.1–1.0μm) in which the S content could be below 1000ppm. No reduction occurred at voltages below 0.5V. Partial reduction was seen at 0.5–0.7V, and converted MoS2to a mixture of MoS2and Mo3S4, or Mo3S4and Mo with the Mo content increasing with the voltage. Cyclic voltammetry of the MoS2powder in a Mo-cavity electrode, together with the electrolysis results, revealed the reduction mechanism to include two steps: MoS2to Mo3S4at −0.28V (potential vs. Ag/AgCl), and then to Mo at −0.43V.