摘要
以Sb2O3为原料,采用配合氧化法制备超细焦锑酸钠。采用X线衍射仪(XRD)、扫描电子显微镜(SEM)和激光粒度分析对焦锑酸钠的结构、形貌和粒度进行表征,并对焦锑酸钠成分进行分析。研究搅拌速度、酒石酸(C4H6O6)和氯化钠(NaCl)用量以及浆化反应时间对焦锑酸钠粒度的影响。研究结果表明:在浆化阶段加入酒石酸将Sb2O3溶解生成配合物,再在碱性条件氧化可显著抑制焦锑酸钠颗粒的长大速度,颗粒粒度从39.62μm降至2.61μm,形貌由四方转变为球形颗粒。焦锑酸钠晶体生长存在沉淀溶解动态平衡。在搅拌速度为400r/min,物质的量比即n(C4H6O6):n(NaCl):n(Sb2O3)=5:12:1,浆化反应时间为120min的条件下,可得到平均粒度为2μm左右,晶形完整的焦锑酸钠产品,锑质量分数为49.02%,纯度大于99%。
Ultrafine sodium pyroantimonate was prepared by combination of complexing and oxidation method with Sb2O3 as raw material. The structure, morphology and particle size of sodium pyroantimonate were characterized by using X-ray diffraction(XRD), scanning electron microscopy(SEM) and laser particle size analysis. The composition of sodium pyroantimonate was analyzed. The effects of stirring rate, amount of tartaric acid and sodium chloride, pulping time on the particle size of sodium pyroantimonate were studied. The results show that the addition of tartaric acid in the pulping stage can dissolve antimony trioxide and get a Sb-complexing solution. The growth rate of sodium pyroantimonate is greatly inhibited by oxidation of this solution in an alkaline medium with the size decreasing from 39.62 μm to 2.61 μm and morphology changing from square to sphere. The growth process of sodium pyroantimonate presents a precipitation and dissolution equilibrium. Under the conditions of stirring rate of 400 r/min, n(C4H6O6): n(NaCl): n(Sb2O3)=5: 12: 1, pulping reaction time of 120 min, sodium pyroantimonate crystal is obtained with a size of 2.0 μm antimony mass fraction of 49.02% and purity greater than 99%.
作者
曹升
杨喜云
李计深
徐徽
石西昌
CAO Sheng;YANG Xiyun;LI Jishen;XU Hui;SHI Xichang(School of Metallurgy and Environment, Central South University, Changsha 410083, China)
出处
《中南大学学报（自然科学版）》
EI
CAS
CSCD
北大核心
2019年第10期2352-2359,共8页
Journal of Central South University:Science and Technology
基金
国家自然科学基金资助项目(51574286)
中国博士后科学基金资助项目(2016M592448)
中南大学博士后基金资助项目(155203)~~
关键词
超细粉体
焦锑酸钠
配合氧化法
粒度控制
ultrafine
sodium pyroantimonate
complexing-oxidation process
particle size control
