“牺牲”阳极法制备金属醇盐

采用金属为“牺牲”阳极 ,在无隔膜电解槽中 ,一步法制备了纳米材料前驱体金属醇盐 :Ti(OEt) 4、Ti(OPr i) 4、Ti(OBu t) 4、Ti(OMe) 2 (acac)、Cu(OEt) 2 、Cu(OBu) 2 、Ni(OEt) 2 和Mg(OEt) 2 ,产物通过元素分析、红外光谱 (FTIR)进行了表征。讨论了影响电合成钛醇盐的关键因素 ,实验表明电极表面粗糙化处理 ,防止阳极钝化 ,温度控制在 5 0～ 6 0℃ ,采用有机季铵溴化物为导电盐 ,可以提高电合成收率。采用合金电极 ,可以有效克服不溶性金属醇盐在阳极的吸附问题 ,并同时合成几种金属醇盐。

Electrochemical Synthesis of Metal Alkoxides Using Sacrificial Anode

Metal alkoxides were directly prepared with pure metal as sacrificial anode in absolute alcohol.The products were characterized by FTIR spectra and elementary analysis.The effects of temperature,conductive additives and trace water on the yield of product were also investigated.The results showed that direct electrochemical preparation of titanium alkoxides had high current efficiency and electrolysis yield.These titanium alkoxides have high purity and can be used directly as precursor of nanometer oxides prepared by Solgel method.The experiments showed that by controlling temperature under 50-60 ℃,selecting R\-4NBr as conductive additives and preventing titanium anode from being passiviated,yield of the product was increased.The use of alloy as anode may be recommended as a technique for the synthesis of alkoxides.This process can run with high current efficiency and high reaction activity.