研究了一种以氯化镁、双氧水和氨水为主要原料,制备过氧化镁的新工艺。通过考察反应原料的滴加顺序及物料比、反应时间、稳定剂种类和用量等对所得产物中过氧化镁含量的影响,分析得出了比较适宜的制备条件:将氯化镁溶液与双氧水溶液混合,滴加氨水反应4 h;Na2HPO4和羟基亚乙基二膦酸(HEDP)作稳定剂;n(MgCl2)∶n(H2O2)∶n(NH3.H2O)=1∶1∶2.5。采用X射线衍射、红外光谱、粒度分布、扫描电镜等对产物进行表征。结果表明,在适宜的制备条件下,所得产物中过氧化镁质量分数可达40%以上,产物在320℃以下不分解。所得产物基本为半结晶状态,形貌不规则,粒度分布范围较宽,中位径为17.62μm。
A new technology of producing magnesium peroxide with magnesium chloride,hydrogen peroxide,and ammonia as main raw materials was studied.By investigating the effects of reactants adding order,amount-of-substance ratio of reactants,reaction time,stabilizer type,and its adding amount etc.,suitable conditions for the preparation of magnesium peroxide were obtained,i.e.magnesium chloride and hydrogen peroxide were mixed firstly,and then ammonia was added,reaction time was 4 h,Na2HPO4 or HEDP were used as stabilizers,and n(MgCl2)∶n(H2O2)∶n(NH3·H2O)=1∶1∶2.5.XRD,FT-IR,SEM,and particle size distribution methods were used to characterize the products.Results showed that under suitable conditions,the mass fraction of magnesium peroxide could reach more than 40%,the products were thermally stable below 320 ℃.The products were not fully crystallized with irregular shapes.The product particles have a relatively wide size distribution range,with a median diameter of 17.62 μm.