“阳极溶解法”制备金属醇盐及其影响因素  

ELECTROCHEMICAL SYNTHESIS OF METAL ALKOXIDES USING SACRIFICING ANODE

作　　者：周幸福[1] 韩爱杰[1] 褚道葆[1] 顾家山[1] 林昌健[2] 林华水[2] 谭建光[2] 

机构地区：[1]安徽师范大学有机化学研究所,安徽芜湖241000 [2]厦门大学材料科学系,福建厦门361005

出　　处：《安徽师范大学学报（自然科学版）》2001年第3期228-230,共3页Journal of Anhui Normal University(Natural Science)

基　　金：安徽省教育厅科研基金 ( 99JL0 0 75 ) ;安徽省自然科学基金 ( 0 0 0 46112 )

摘　　要：采用金属为“牺牲”阳极 ,在无隔膜电解槽中 ,一步法制备金属醇盐 :Ti(OEt) 4、Ti(OPr -i) 4、Ti(OMe) 4(acac)、Cu(OEt) 2 、Cu(OBu) 2 、Ni(OEt) 2 和Mg(OEt) ,产物通过元素分析、红外光谱进行表征 .实验表明电极表面粗糙化处理 ,防止阳极纯化 ,温度控制在 5 0 - 60℃之间 ,采用有机溴化胺电导盐 ,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 ,从而提高反应的电流效率 .Metal alkoxides were directly prepared using pure metal as sacrificing anode in absolute alcohol. Metal alkoxides were characterized by FTIR spectra and element analysis. The effects of temperature,conductive additives,trace water on product yield were also investigated. The results showed that the direct electrochemical preparation of metal alkoxides had high current efficiency and electrolysis yield. These metal alkoxides have high purity and can be directly used as precursor of nanometer oxides prepared by Sol-gel method. The experiments showed that controlling temperature under 50-60℃, selecting R 4NBr as conductive additives and preventing titanium anode from being passiviated can improve product yield. Using alloy as anode may be recommended as a technique for the synthesis of alkoxides, this process can run in sufficiently high current efficiency and high reaction activity.

关 键 词：金属醇盐 有机电合成 阳极溶解法 “牺牲”阳极 电效效率 纳米材料 

分 类 号：O627[理学—有机化学] O646.542[理学—化学]