(吉首大學 化學化工學院，吉首 416000)
摘 要: 采用硫酸錳兩步法合成高純四氧化三錳，研究水解物的生成及洗滌條件對水解物及四氧化三錳中硫酸根含量的影響。測定不同加料方式、氨錳比、硫酸錳濃度、反應溫度、氨水滴加速度條件下生成的水解物及其四氧化三錳產(chǎn)品的硫酸根含量，并對水解物分別使用稀氨水硝酸銨溶液和水洗滌，測定勻漿及淋洗兩種洗滌方式下水解物的硫酸根含量。結(jié)果表明：在硫酸錳濃度0.5 mol/L、溫度60 ℃、氨水滴加時間20 min、氨錳比為3:1的條件下，采用向硫酸錳溶液中滴加稀氨水的加料方式，四氧化三錳產(chǎn)率可達86.1%；采用勻漿洗滌方法能明顯降低水解物的硫酸根含量，其效果優(yōu)于淋洗方法；使用2%稀氨水勻漿洗滌兩次所得四氧化三錳的硫酸根含量可降低至0.09%。
關(guān)鍵字: 硫酸錳；四氧化三錳；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
