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铁道科学与工程学报

JOURNAL OF RAILWAY SCIENCE AND ENGINEERING

Vol. 18    No. 1    January 2008

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Preparation of high-purity tantalum ethoxide by vacuum distillation
YANG Sheng-hai(杨声海)1, CHEN Yong-ming(陈永明)1, YANG Hai-ping(杨海平)1,LIU Yin-yuan(刘银元)1, TANG Mo-tang(唐谟堂)1, QIU Guan-zhou(邱冠周)2

1.School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China;2. School of Minerals Processing and Bioengineering, Central South University, Changsha 410083, China

Abstract: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%.

 

Key words: tantalum ethoxide; distillation; FTIR

ISSN 1672-7029
CN 43-1423/U

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