摘要
目前90%以上的稀土均采用溶剂萃取的方式进行冶炼分离,其中常用的萃取剂为HEH（EHP）。由于萃余液中萃取剂HEH（EHP）含量较低,无法直接检测其含量。采用硝酸和高氯酸高温分解的方法,将酸性磷类萃取剂HEH（EHP）中的磷全部转化为正磷酸盐,用电感耦合等离子发射光谱法（ICP-AES）测定样品中的磷含量,从而通过测量磷含量推断得到萃余液中L^-1萃取剂含量,建立了一种简单快捷高效的处理和测试样品的方法。试验结果表明,最佳的分析谱线波长为213.618 nm,该方法测试检出限达到0.06 mg·L^-1,磷加标回收率达到97.5%～103.0%,同时样品的测试标准偏差控制在5%以内。通过对提纯后的HEH（EHP）进行称重消解测试分析发现,采用硝酸和高氯酸混合分解的方法可以将有机磷完全转化为正磷酸盐,从而验证了本方法的可行性。此方法将大大提高萃余液中萃取剂含量的分析速度和测量精度,为稀土冶炼分离过程中萃余液中萃取剂含量的分析检测提供了技术保障。
At present,the most commonly used extractant is HEH（EHP）. However,the content of the HEH（EHP） extractant remained in raffinate is too low to be detected directly after extraction. In this paper,a new method was proposed to solve this problem.Phosphorus extractant HEH（EHP） was decomposed by nitric acid and perchloric acid,and all organic phosphorus was converted to orthophosphate,which was measured by ICP-AES. The content of extractant in the raffinate was deduced by measuring the phosphorus concentration. A simple,rapid and efficient method for treating and testing the phosphorus was established. Results showed that the optimal analytical wavelength was 213. 618 nm,the detection limit of this method was 0. 06 mg·L^-1,the recovery rate of phosphorus could reach 97. 5% ～ 103. 0%,and the standard deviation of the sample was less than 5%. Through weighing and digestion of the purified HEH（EHP）,it was found that the nitric acid and perchloric acid could completely convert organic phosphorus into orthophosphate by the method of mixed decomposition,which could prove the feasibility of this method. The analysis efficiency and measurement accuracy were improved greatly. This method provided technique guarantee for rare earth smelting separation and extraction process.
作者
董金诗
冯宗玉
孟祥龙
薛倩楠
王良士
黄小卫
Dong Jinshi;Feng Zongyu;Meng Xianglong;Xue Qiannan;Wang Liangshi;Huang Xiaowei(National Engineering Research Center for Rare Earth Materials, General Research Institute for Nonferrous Metals, Beijing 100088, China;Grirem Advanced Materials Co., Ltd., Beijing 100088, China)
出处
《稀有金属》
EI
CAS
CSCD
北大核心
2018年第6期663-667,共5页
Chinese Journal of Rare Metals
基金
国家科技支撑计划项目(2015BAB16B01)资助
