氟化法深度脱除业硫酸锰中钙镁的研究.docVIP

doi： doi：10.3969/j.issn.1007-7545.2018.07.001 何婷婷，钱磊，崔静贤，粟海锋 （广西大学 化学化工学院，南宁 530004） 摘要：使用氟化铵为脱除剂，研究了工业硫酸锰中钙、镁杂质的深度除杂工艺。通过正交试验和单因素试验研究了反应时间、氟化铵过量系数、反应温度和pH对钙、镁脱除效果的影响。结果表明，影响钙和镁脱除效果的因素依次为氟化铵过量系数、反应温度、反应时间和pH。在氟化铵过量系数为2，反应温度90 ℃，反应时间60 min和pH=4.5的条件下，钙、镁脱除率分别达到99.18%和97.05%。在反应后期加入适量的硫酸铝，不仅可以强化沉淀效果、改善过滤性能，还可以去除一部分溶液中残留的氟离子。 关键词：硫酸锰；钙；镁；氟化铵；除杂 中图分类号：TF803.2+5 文献标志码：A 文章编号：1007-7545（2018）07-0000-00 Deep Removal of Ca and Mg from Industrial Manganese Sulfate with Fluorination Precipitation HE Ting-ting, QIAN Lei, CUI Jing-xian, SU Hai-feng (School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China) Abstract：Purification of Ca and Mg in industrial manganese sulfate was studied with ammonium fluoride as precipitant. The influences of reaction time, ammonium fluoride overdose, reaction temperature, and pH value on purification rates of Ca and Mg were investigated through orthogonal test and single factor experiment. The results show that influence on purification rates of Ca and Mg is sequenced as ammonium fluoride overdose, reaction temperature, reaction time and pH value. Ca and Mg removal rate is 99.18% and 97.05% respectively under the conditions including ammonium fluoride overdose of 2, reaction temperature of 90 ℃, reaction time of 60 min, and pH value of 4.5. Addition of proper amount of aluminum sulfate can not only enhance precipitation effect and improve filtration performance, but also remove part of fluoride ions remaining in solution. Key words: manganese sulfate; calcium; magnesium; ammonium fluoride; purification 硫酸锰是重要的锰系产品，随着国内三元材料等产业的发展，高纯硫酸锰具有良好的发展前景[1]。然而，使用低品位锰矿浸出生产的硫酸锰产品杂质较多，无法满足市场的需要。在这些杂质中，钙和镁最难去除。近年来，国内外学者对此进行了较多的研究。袁飞等[2]从低锰镁质量比溶液中结晶分离锰镁，发现溶液中锰镁质量比对锰和镁的结晶分离影响较大，锰镁质量比越小，二者越难分离。刘洪刚等[3]用30%的P507加70%的磺化煤油作为萃取剂来萃取钙镁离子，镁、钙的萃取率分别为72.06%和48.97%，锰的损失为6.35%。谭力铭等[4]以Versatic10为萃取剂从含钙、镁、钾、钠的模拟硫酸锰浸出液中选择性萃取锰，产物中钙、镁、钾、钠的含量均小于15 mg/L，取得了较好的分离效果。LIN等[5]采用碳酸共沉淀法来分离锰和钙镁，在最优条件下，碳酸锰产物中含Mn 44.62%、Ca 0.25%和Mg 0.08%。张彭汝等[6]研究了以MgF2晶种为成核剂的