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,oi...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%.展开更多
基金Project(50404011)supported by the National Natural Science Foundation of ChinaProject(20040350187)supported by the Postdoctoral Science Foundation of ChinaProject(2007AA03Z425)supported by the Hi-Tech Research and Development Program of China
文摘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%.
