(1. 北京科技大学 土木与环境工程学院,北京 100083;
2. 中国科学院 过程工程研究所,生化工程国家重点实验室,北京 100190)
摘 要: 研究氯化锰与石灰乳制备四氧化三锰,并采用正交实验考察石灰乳浓度为1 mol/L时,Mn2+浓度、反应温度、石灰乳加料速度对氢氧化锰纯度的影响。正交实验结果表明,氯化锰浓度为 0.5 mol/L、反应温度为 80 ℃、加料速度为6 mL/min时,氢氧化锰中锰含量可达60%以上,初级产品四氧化三锰中锰含量为70.42%。X射线衍射、化学多元素和红外分析显示,初级产品四氧化三锰中的主要杂质为氧化钙和碱式氯化锰。碱式氯化锰可通过氢氧化钠溶液处理而去除。热力学计算和实验结果表明,水热法可同时除去杂质氧化钙和碱式氯化锰,最终产品锰含量可达71.27%。
关键字: 石灰乳;碱式氯化锰;四氧化三锰;水热法
(1. School of Civil and Environment Engineering, University of Science and Technology Beijing, Beijing 100083, China;
2. State Key Laboratory of Biochemical Engineering, Institute of Process Engineering,
Chinese Academy of Sciences, Beijing 100190, China)
Abstract:Manganese tetroxide was prepared with manganese chloride and lime milk. The influences of manganese ion concentration, reaction temperature and feeding speed were investigated through orthogonal experiments when the concentration of lime milk is 1 mol/L. The results show that the manganese in manganese hydroxide is above 60% when the feeding speed is 6 mL/min with manganese ion concentration of 0.5 mol/L and at 80 ℃. The content of manganese in the product is 70.42 %. The results of X-ray diffraction, chemical multi-element and infrared analysis show that calcium oxide and basic manganese chloride are main impurities in the manganese tetroxide primary products. Basic manganese chloride can be removed by the processing of sodium hydroxide solution. The thermodynamic calculations and experimental results indicate that the hydrothermal method can eliminate the impurities of calcium oxide and basic manganese chloride simultaneously, and the content of final products manganese is up to 71.27%.
Key words: lime milk; basic manganese chloride; manganese tetroxide; hydrothermal method