电化学合成乙醇铌工艺研究

Technology Research on Electrochemical Synthesis of Niobium Ethoxide

用金属铌作阳极电化学直接合成了乙醇铌,用拉曼光谱、红外光谱和元素分析对产品进行了表征。实验研究了导电剂的种类与浓度、乙醇含水量、电流密度、极距和电解液温度对电化学合成乙醇铌的影响,确定最佳工艺条件为:乙醇经除水处理,导电剂(C2H5)4NBr浓度为0.04mol/L,极距2.5cm,电流密度300～330A/m2,电解液处在沸腾状态,合成时间76～80h,在此最佳条件下,电化学合成的电流效率大于95%,产品中铌的直收率大于96%。

Niobium ethoxides, directly prepared by electrochemical method using metal niobium as anode, were characterized by Raman spectra, FT-IR spectra and element analysis. The effect of conductive agents, residual moisture, current density, polar distance and electrolyte temperature on the synthesis were investigated by experiments. The technology were optimized as dewatered ethanol, （C2H5）4NBr concentration 0.04 mol/L, polar distance 2.5 cm, current density 300-330 A/m2, boiling temperature and synthesis time 76-80 h. The current efficiency is over 95 % and direct niobium transform rate is over 96 % at the optimized conditions.