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研究了以Sc2O3为原料,盐酸回流溶解后与NaCl,KCl,NH4Cl溶液混合,经蒸发浓缩、结晶、真空预脱水,再在氩气保护下分段升温脱水、升华除去过量NH4Cl后制备ScCl3 NaCl KCl熔盐的新工艺。研究表明,添加NH4Cl后加热脱水时,NH4Cl分解产生的HCl气体能抑制Sc Cl3水合物加热过程中的水解,溶解产生的水不溶性钪,从而有效地防止了Sc2O3等水不溶化合物的生成。制备的ScCl3 NaCl KCl熔盐脱水完全、水不溶性钪含量很低,能满足熔盐金属热还原法制备金属钪及铝钪中间合金对熔盐原料的要求。
In this paper, Sc2O3 was used as raw material, hydrochloric acid was mixed with NaCl, KCl and NH4Cl solution after refluxing and dissolving, then concentrated by evaporation, crystallized, pre-dehydrated in vacuum, and then heated and dehydrated by fractional heating under argon to sublime and remove excess NH4Cl to prepare ScCl3 NaCl KCl Molten salt of the new technology. The results show that when NH4Cl is added and heated to dehydrate, the HCl gas produced by the decomposition of NH4Cl can inhibit the hydrolysis and dissolution of the sc-Cl3 hydrate during the heating process, thus effectively preventing the formation of water-insoluble compounds such as Sc2O3. The preparation of ScCl3 NaCl KCl molten salt dehydration is complete, water-insoluble scandium content is very low, to meet the molten salt metal thermal reduction preparation of metal scandium and aluminum scandium master alloy molten salt raw material requirements.