“牺牲”阳极法直接电化学合成5-二乙基胺钽  

Direct electrosynthesis of pentakis(diethylamido)tantalum using sacrificing anode

作　　者：陈胜龙[1] 杨建广[1] 高亮[1] 刘小文[1] 吴玉山[1] 杨济豪[1] 

机构地区：[1]中南大学冶金科学与工程学院,湖南长沙410083

出　　处：《中南大学学报（自然科学版）》2011年第11期3251-3255,共5页Journal of Central South University:Science and Technology

基　　金：国家自然科学基金资助项目(50804056;51174237)

摘　　要：采用金属钽板为阳极,不锈钢板为阴极,以四丁基溴化铵为导电剂,溶解到添有某一惰性溶剂AB的二乙胺中电解,直接电化学合成5-二乙基胺钽(PDEAT),研究支持电解质的种类与浓度、电解液的温度、阴阳极距以及槽电压的影响。选取最佳合成条件为:四丁基溴化铵浓度0.04 mol/L,温度为50℃,极距为0.4 cm,槽电压为50 V,电合成的产品在5 kPa的压力下减压蒸馏分离得到粗级产品,采用红外光谱对产品进行初步的表征,说明5-二乙基胺钽能够采用直接电化学合成法制备。Pentakis（diethylamido）tantalum（Ⅴ） was synthesized by electrochemical reactions of diethylamine in which diluted solvent of AB at sacrificial tantalum anode in the presence of tetrabutylammonium bromide is used as a conductive additive.The effects of additive species,additive concentration,temperature,anode to cathode distance and cell voltage on the electrochemical synthesis of PDEAT using sacrificing anode method were investigated.The optimum conditions are tetrabutylammonium bromide 0.04 mol/L,temperature 50 ℃,distance 0.4 cm and cell voltage 50 V.The crude products are isolated by reduced pressure distillation under 5 kPa.These samples are characterized by Fourier transform infrared spectra（FT-IR）,The results show that PDEAT can be prepared by direct electrochemical synthesis.

关 键 词：电化学合成 5-二乙基胺钽 红外光谱 二乙胺 四丁基溴化铵 

分 类 号：TG111.3[金属学及工艺—物理冶金]