Preparation of high-purity tantalum ethoxide by vacuum distillation  

作　　者：杨声海 陈永明 杨海平 刘银元 唐谟堂 邱冠周 

机构地区：[1]School of Metallurgical Science and Engineering,Central South University [2]School of Minerals Processing and Bioengineering

出　　处：《中国有色金属学会会刊：英文版》2008年第1期196-201,共6页Transactions of Nonferrous Metals Society of China

基　　金：Project(50404011)supported by the National Natural Science Foundation of China;Project(20040350187)supported by the Postdoctoral Science Foundation of China;Project(2007AA03Z425)supported by the Hi-Tech Research and Development Program of China

摘　　要：Effects of reflux ratio,water addition and content of water in ethanol on the purity and yield of tantalum ethoxide during vacuum distillation were investigated under the operational conditions of pressure of 1 kPa,oil bath temperature of 210-230 ℃,and outlet temperature of 190 ℃.The condensate sample was characterized by FTIR,1H-NMR spectroscopy and Raman spectra,respectively.The contents of tantalum,carbon and hydrogen in the sample were also determined with elemental analysis instrument.The obtained results consistently demonstrate that the condensate is tantalum ethoxide.The content of impurity,such as Al,As,Ca,Co,Cr,Cu,Fe,K,Mg,Mn,Mo,Na,Ni,Pb,Sn,Ti,V and Zn,in tantalum ethoxide is less than 0.000 05%,while Nb content is less than 0.000 5%.The content of impurities in tantalum ethoxide sample excels that of Epichem Group's requirement for Ta(OC2H5)5 of 99.999%.Effects of reflux ratio, water addition and content of water in ethanol on the purity and yield of tantalum ethoxide during vacuum distillation were investigated under the operational conditions of pressure of 1kPa, oil bath temperature of 210-230 ℃, and outlet temperature of 190℃. The condensate sample was characterized by FTIR, 1↑H-NMR spectroscopy and Raman spectra, respectively. The contents of tantalum, carbon and hydrogen in the sample were also determined with elemental analysis instrument. The obtained results consistently demonstrate that the condensate is tantalum ethoxide. The content of impurity, such as Al, As, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Ni, Pb, Sn, Ti, V and Zn, in tantalum ethoxide is less than 0.000 05%, while Nb content is less than 0.000 5%. The content of impurities in tantalum ethoxide sample excels that of Epichem Group＇s requirement for Ta（OC2H5）5 of 99.999%.

关 键 词：高纯度乙醇钽 真空蒸馏 杂质 化学制剂 

分 类 号：TF841.6[冶金工程—有色金属冶金]