(吉首大学 化学化工学院，吉首 416000)
摘 要: 采用硫酸锰两步法合成高纯四氧化三锰，研究水解物的生成及洗涤条件对水解物及四氧化三锰中硫酸根含量的影响。测定不同加料方式、氨锰比、硫酸锰浓度、反应温度、氨水滴加速度条件下生成的水解物及其四氧化三锰产品的硫酸根含量，并对水解物分别使用稀氨水硝酸铵溶液和水洗涤，测定匀浆及淋洗两种洗涤方式下水解物的硫酸根含量。结果表明：在硫酸锰浓度0.5 mol/L、温度60 ℃、氨水滴加时间20 min、氨锰比为3:1的条件下，采用向硫酸锰溶液中滴加稀氨水的加料方式，四氧化三锰产率可达86.1%；采用匀浆洗涤方法能明显降低水解物的硫酸根含量，其效果优于淋洗方法；使用2%稀氨水匀浆洗涤两次所得四氧化三锰的硫酸根含量可降低至0.09%。
关键字: 硫酸锰；四氧化三锰；除硫
（College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000, China）
Abstract:The effects of preparation and rinsing conditions for hydrolysate on sulfate content of MnSO4 were investigated in the process of high-purity Mn3O4 prepared by two-step method from MnSO4. The sulfate contents of hydrolysate and Mn3O4 prepared under different feeding sequences, ratio of ammonia to manganese, concentration of manganese sulfate solution, reaction temperature and feeding rate of ammonia solution were determined. The hydrolysates were washed with ammonia, ammonia nitrate solution and water, respectively, and their sulfate contents of hydrolysate washed by homogenate and rinsing method were determined. The results show that, under the following conditions of MnSO4 concentration of 0.5 mol/L, temperature of 60 ℃，ratio of ammonia to manganese of 3:1, feeding time of 20 min, using the feeding sequence of adding ammonia to manganese solution, the yield of Mn3O4 is 86.1%. Using homogenate washing method can sharply decrease the sulfate content of hydrolysate, which is better than using rinsing method. The sulfate content of Mn3O4 washed with 2% ammonia for 2 times can lower to 0.09%.
Key words: manganese sulfate; trimanganese tetroxide; sulfur removal
