硫酸锰溶液碱化沉淀—焙烧法制备Mn_3O_4

Preparation of Mn_3O_4 by Alkaline Precipitation-Calcination Process Using MnSO_4 Solution

针对传统Mn3O4生产过程中存在工艺控制复杂和污染物排放量大的问题,结合传统液相法和焙烧法的优点,提出了先用NaOH滴加含有分散剂十二烷基硫酸钠(SDS)的硫酸锰溶液制备四氧化三锰前驱体,再焙烧前驱体制备Mn3O4,用SEM、XRD对产物进行表征。试验结果表明:在SDS投加量1.5g/L、反应温度60℃、反应时间30min和搅拌转速300r/min条件下,可得到粒径约100nm、大小分布均匀的纳米级前驱体颗粒,其主要由Mn(OH)2、MnOOH和Mn3O4组成;前驱体焙烧制备Mn3O4最佳温度为1 000℃,此时可得到呈四方尖晶石结构、粒径约500nm、颗粒大小均匀的Mn3O4产品。

The traditional preparation technology for Mn3 O4 has the problems of difficult process control and high pollutant .Combined with the advantages of the traditional liquid phase method and roasting method ,the new method that preparation of Mn3 O4 precursor using MnSO4 solution with despersant SDS by adding NaOH and preparation of Mn3 O4 through roasting the precursor was presented .The SEM and XRD analysis results show that under the experimental conditions for preparation of precursor of 1 .5 g/L SDS ,30 min reaction time ,60 ℃ reaction temperature and 300 r/min agitation rate ,uniform size particles about 100 nm can be obtained .The precursor composes of Mn（OH）2 ,MnOOH and Mn3 O4 .The best roasting temperature for preparing Mn3 O4 is 1 000 ℃ ,and Mn3 O4 product has tetragonal morphology with particle size of about 500 nm .