Direct Electrochemical Desulfurization of Solid Sb2S3 to Antimony Powders in Deep Eutectic Solvent
Direct Electrochemical Desulfurization of Solid Sb2S3 to Antimony Powders in Deep Eutectic Solvent
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低共熔溶剂中固体Sb2S3直接电化学脱硫制锑粉
DOI：
10.1149/2.0041914jes
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发表时间：
2019-10
影响因子：
3.9
通讯作者：
Cunying Xu
中科院分区：
文献类型：
--
作者：
Zhiwei Wang;Juanjian Ru;Jiaojiao Bu;Yixin Hua;Yuan Zhang;Cunying Xu
在353 K下，以氯化乙二醇为电解液，采用直接电还原法制备了锑粉和纳米硫粉。Sb 2S 3在铂粉空腔微电极上的循环伏安曲线表明，Sb 2S 3电化学脱硫是通过三电子转移一步完成的。恒压电解表明，Sb 2S 3在16 h内可完全转化为金属Sb和硫磺，阴极电流效率约为50.64%。ESI-MS分析表明，除直接脱硫过程外，还存在[SbCl 4]−→ Sb 0的电沉积过程，并形成了四配位的络合阴离子[SbCl 4]−。溶解的Sb（III）离子可以被还原并沉积在Sb颗粒上，形成更大的处于更稳定状态的半球形颗粒，其看起来像蜗牛壳来包裹这些Sb颗粒。无定形硫粉末相互间形成致密的团聚体，形成网状结构，形貌为直径14-25 nm的不规则球形。分析了Sb 2S 3粉末的电脱硫过程，并给出了示意图。这一发现为在近室温、流程短、无SO2排放的条件下，实现从辉锑矿资源中提取锑的绿色提取提供了可能。
Antimony (Sb) powders and sulfur nanoparticles have been prepared by direct electroreduction of solid Sb 2 S 3 in ChCl-EG DES at 353 K. Cyclic voltammogram of Sb 2 S 3 on Pt-powder cavity microelectrode demonstrates that the electrochemical desulfurization of Sb 2 S 3 to metallic Sb is a one-step process through three-electron transfer. Constant voltage electrolysis indicates that Sb 2 S 3 can be completely transformed into metallic Sb and sulfur for 16 h, and the cathodic current efficiency is about 50.64%. Besides, ESI-MS analysis implies that four-coordinated complex anions [SbCl 4]− are formed and the electrodeposition of [SbCl 4]−→ Sb 0 also exists simultaneously except for the mainly direct desulfurization process. Dissolved Sb (III) ions can be reduced and deposited at Sb grains to form larger hemispherical particles in a more stable state, which looks like a snail shell to encapsulate these Sb grains. In addition, amorphous sulfur powders are densely agglomerated with each other to establish a network structure and the morphology is irregularly globular with diameters of 14–25 nm. The electro-desulfurization process of Sb 2 S 3 powders has been analyzed and a schematic illustration is also proposed. This finding provides a possible way for green extraction of Sb from stibnite resources in DESs at near room temperature with short process and emission-free SO 2.
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