Cui Xi, Zhang Wenzheng, Ji Rui, Yang Mingliang, Wang Shichao, Qu Tao
Key Laboratory for Nonferrous Vacuum Metallurgy of Yunnan Province, Kunming University of Science and Technology, Kunming 650093, China.
National Engineering Research Center of Vacuum Metallurgy, Kunming University of Science and Technology, Kunming 650093, China.
Materials (Basel). 2024 Apr 24;17(9):1960. doi: 10.3390/ma17091960.
With the rapid development of high and new technology, rubidium and its compounds show broad application prospect and market demand with their unique characteristics. At present, the production of rubidium metal is mainly prepared by calcium thermal reduction of rubidium chloride. Rubidium metal obtained by reduction requires multi-step vacuum distillation to obtain high-purity rubidium metal. The purity of rubidium metal depends on the purity of the raw material rubidium chloride. Rubidium metal is relatively active and is easy to oxidize and explode in air. Therefore, a method combining vacuum decomposition and vacuum distillation to reduce impurity elements in rubidium chloride from raw materials is proposed in this paper. The experimental results show that under the conditions of pressure of 5-10 Pa, distillation temperature of 823 K and vacuum distillation time of 60 min, the contents of Si and Zn impurities are reduced from 1206 mg/kg and 310 mg/kg to less than 0.1 mg/kg, and the removal rates are 99.99% and 99.97%, respectively. Rubidium chloride has almost no loss, and through one-step vacuum distillation, the impurity elements silicon and zinc can be deeply removed, reducing the flammability and explosiveness, high cost, long process and other problems caused by the subsequent preparation of high-purity rubidium metal.
随着高新技术的飞速发展,铷及其化合物以其独特的性能展现出广阔的应用前景和市场需求。目前,金属铷的生产主要采用氯化钙热还原氯化铷的方法。还原得到的金属铷需经过多步真空蒸馏才能获得高纯度的金属铷。金属铷的纯度取决于原料氯化铷的纯度。金属铷化学性质相对活泼,在空气中易氧化爆炸。因此,本文提出一种将真空分解与真空蒸馏相结合的方法,以降低原料氯化铷中的杂质元素。实验结果表明,在压力为5 - 10 Pa、蒸馏温度为823 K、真空蒸馏时间为60 min的条件下,硅和锌杂质含量从1206 mg/kg和310 mg/kg降至0.1 mg/kg以下,去除率分别为99.99%和99.97%。氯化铷几乎无损失,通过一步真空蒸馏可深度去除杂质元素硅和锌,减少了后续制备高纯度金属铷过程中存在的易燃易爆、成本高、流程长等问题。