锑酸锂与六氟锑酸锂制备新技术集成  

An integration of new technologies for preparation of lithium antimonite and lithium hexafluoroantimonate

作　　者：刘伟锋 唐攒浪 陈霖 张杜超 杨天足 LIU Weifeng;TANG Zanlang;CHEN Lin;ZHANG Duchao;YANG Tianzu(School of Metallurgy and Environment, Central South University, Changsha 410083, China)

机构地区：[1]中南大学冶金与环境学院

出　　处：《中南大学学报（自然科学版）》2019年第8期1768-1777,共10页Journal of Central South University:Science and Technology

基　　金：国家重点研发计划项目(2018YFC1901604);国家自然科学基金资助项目(51404296);国家留学基金委访问学者项目(201806375047);中南大学中央高校基本科研业务费专项资金资助项目(1053320170238)~~

摘　　要：为了改进锑酸锂制备的传统工艺,提出间接锂盐法、直接锂盐法和钾盐法3种新技术制备锑酸锂,即以Sb2O3为原料在水溶液中氧化后制备得到锑酸锂晶体;以LiSb(OH)6和Sb2O3为原料,分别经过锑酸锂法和六氟锑酸法制备得到LiSbF6溶液,再经过浓缩、结晶和干燥后得到LiSbF6晶体。研究结果表明:锑酸锂产品中Sb(Ⅲ)的质量分数极低(<0.01%),锂与锑的化学配比精准,产品纯度高(≥98%),微观形貌为分布均匀的六边形层状和六方柱2种结构。六氟锑酸锂产品物相组成为单一的LiSbF6相,锂、锑和氟的化学配比精准,产品纯度高(≥98%),在550~850cm^-1的波数范围内存在SbF^-6的特征峰。To improve the traditional preparation process of LiSb(OH)6 crystal, three new methods including indirect lithium salt, direct lithium salt and potassium salt were proposed to synthesize LiSb(OH)6 crystal by the oxidation of Sb2O3 in solution. LiSb(OH)6 and Sb2O3 were used as the raw materials, and LiSbF6 solutions were prepared by lithium antimonate and hexafluoroantimonic acid methods. Then, the crystalline LiSbF6 was obtained from these solutions after concentration, crystallization and drying procedures. The results show that the mass fraction of Sb(Ⅲ) is fairly low (<0.01%), the molar ratio between Li and Sb is accurate, and the purity of LiSb(OH)6 also exceeds 98%. Furthermore, these LiSb(OH)6 crystals uniformly distribute in the form of hexagonal layered structure and hexagonal prism structure. Synthesized LiSbF6 crystals are in single-phase with good crystallinity. The molar ratio among Li, Sb and F is accurate, which indicates that the purity of LiSbF6 crystals is extremely high (≥98%). Moreover, there exists characteristic vibrational peaks of SbF^-6 in the wavenumber range of 550~850 cm^-1 in these LiSbF6 crystals.

关 键 词：锑白 锑酸锂 六氟锑酸锂 

分 类 号：TF818[冶金工程—有色金属冶金]