(1. 昆明理工大學(xué) 材料與冶金工程學(xué)院， 昆明 650093；
2. 云南冶金集團(tuán)總公司技術(shù)中心，昆明 650031)
摘 要: 針對粗銻精煉過程中銻鉍難以分離的技術(shù)難點(diǎn)，采用H2SO4-NH4F-SbF3電解液體系進(jìn)行高鉍粗銻電解精煉除鉍，考察溫度、電流密度及添加劑對除鉍的影響。通過掃描電鏡(SEM)分析，研究添加劑對陰極銻沉積形貌的影響。獲得水溶液電解精煉除鉍的最佳工藝條件為：室溫(25 ℃)，電流密度為400 A/m2，異極距為50 mm，草酸加入量為10 g/L，電解周期為24 h。實驗結(jié)果表明，銻電結(jié)晶按螺旋位錯生長機(jī)理進(jìn)行，其晶體呈三角棱錐結(jié)構(gòu)；當(dāng)草酸含量在適當(dāng)范圍之內(nèi)時，銻鍍層的生長機(jī)理無明顯變化。
關(guān)鍵字: 銻；電解精煉；鉍；草酸
（1. Faculty of Materials and Metallurgical Engineering, Kunming University of Science and Technology,
Kunming 650093, China;
2. Technique Center of Yunnan Metallurgy Co. Ltd, Kunming 650031, China）
Abstract:It is difficult to separate bismuth and antimony in the process of crude refining. The electro refining of high-bismuth antimony was studied by using ammonium fluoride-antimony sulphate electrolyte system. The influences of temperature, current density and additives on bismuth removal from crude antimony were discussed. The effect of additives on morphologies of cathodic deposition layer was investigated by scanning electron microscopy (SEM). Optimum process parameters, namely, temperature of 25 ℃, current density of 400 A/m2, distance between anode and cathode of 50 mm, oxalic acid dosage of 10 g/L and electrolytic period of 24 h, were ascertained. The result shows that electrocrystallization of antimony follows the screw dislocation growth mechanism with a trigonal pyramids structure, and addition of oxalic acid to electrolyte has no remarkable change in it if the dosage is appropriate.
Key words: antimony; electro refining; bismuth; oxalic acid
