Investigation on effect of the stratified sampling mode on determination results of physical and chemical index of mixed RECl3 solution produced during rare earth carbonate production by ammonium bicarbonate precipitation method
SHEN Menglin1,2, ZHAO Wenyi1,2, LI Huachang3, WANG Yan1, WANG Dongjie*3
1. National Key Laboratory for Research and Comprehensive Utilization of Rare Earth Resources in Baiyun Obo, Baotou Research Institute of Rare Earths, Baotou 014030, China; 2. School of Chemical Engineering & Technology, Tianjin University, Tianjin 300350, China; 3. BGRIMM Technology Group, Beijing 102600, China
Abstract：The extraction and separation of rare earths require a series of processes such as sulfuric acid roasting, water leaching, extraction, back extraction, and ammonium bicarbonate precipitation. Among them, the mixed RECl3 solution is an important intermediate product in the rare earth industry line. The physical and chemical indexes of mixed rare earth solution, including rare earth oxide (REO) concentration, the ratio of single rare earth to the total rare earth, and density, are the key parameters to evaluate the quality of mixed RECl3 solution products. According to the national standard analysis methods and other approaches including X-ray fluorescence spectrometry (XRF), inductively coupled plasma atomic emission spectrometry (ICP-AES) and gravimetry, the effect of the stratified sampling mode on the determination results of REO concentration, the ratio of single rare earth to the total rare earth, and the solution density in mixed RECl3 solution stored under certain environmental condition was investigated. The changing curve of REO concentration and density was plotted by varying the storage time. It was found that the difference of determination results of samples with different stratified sampling mode increased with increasing the storage time of mixed RECl3 solution. The influence factors of sampling depth of mixed RECl3 solution on the determination results was briefly discussed. The mixed RECl3 solution was sampled at uniform intervals from surface to bottom for determination. The results of REO concentration and density showed an increasing trend. While the ratio of light rare earth to the total rare earth showed a decreasing trend, and the ratio of heavy rare earth to the total rare earth showed an increasing trend. The variation trend of REO mass concentration with REO concentration range difference in mixed RECl3 solution within certain storage time were investigated. It was shown that the determination results of REO concentration changed slowly when its mass concentration was less than 50 g/L or higher than 250 g/L. When REO mass concentration was in range of 100-200 g/L, the determination results of REO concentration changed fast. The basic theory for the influence of stratified sampling mode on determination results was deeply analyzed. This study could be used to guide the quality control of mixed RECl3 solution in rare earth production industry. It had important guiding significance for normalizing the sampling operation of mixed RECl3 solution.
申孟林, 赵文怡, 李华昌, 王彦, 王东杰. 分层取样方式对碳酸氢铵沉淀法生产碳酸稀土过程混合RECl3溶液理化指标检测结果的影响研究[J]. 冶金分析, 2022, 42(6): 57-63.
SHEN Menglin, ZHAO Wenyi, LI Huachang, WANG Yan, WANG Dongjie. Investigation on effect of the stratified sampling mode on determination results of physical and chemical index of mixed RECl3 solution produced during rare earth carbonate production by ammonium bicarbonate precipitation method. , 2022, 42(6): 57-63.
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