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分析了氯化钪易水解生成ScOCl的机制,提出了抑制ScOCl生成的研究方案:在熔盐中加入氯化铵,从而抑制了无水氯化钪熔盐脱水过程中氯化钪的水解,制定了脱除氯化铵和剩余结晶水的新工艺。对无水氯化钪熔盐制备过程中脱氯化铵和剩余结晶水阶段的温度、氯化铵用量、时间、升温速度和惰性气体流量等因素对钪水解率的影响进行了试验研究。得出此阶段的最佳工艺条件为:温度400℃,氧化钪与氯化铵质量比1∶1.5(氧化钪与辅盐质量比1∶5.4),时间120min,升温速度10℃.min-1,惰性气体流量5L.min-1。
The mechanism of ScCIl scavenging by scandium chloride was analyzed, and the research project of ScOCl inhibition was proposed. Ammonium chloride was added to the molten salt to restrain the scandium chloride hydrolysis during the dehydration of anhydrous scandium chloride A new process for removal of ammonium chloride and residual water of crystallization. The effects of factors such as the temperature of ammonium chloride removal and residual crystallization water, the amount of ammonium chloride, the time, the heating rate and the inert gas flow rate on the scandium hydrolysis rate during the preparation of anhydrous scandium chloride molten salt were studied. The optimum technological conditions of this stage were as follows: the temperature was 400 ℃, the mass ratio of scandium oxide to ammonium chloride was 1: 1.5 (the mass ratio of scandium oxide to the auxiliary salt was 1: 5.4), the time was 120min and the temperature was increased by 10 ℃ .min-1 , Inert gas flow 5L.min-1.