电化学方法合成铅、钛金属醇盐

Synthesis of Lead and Titanium Alkoxides by Electrochemistry

通过改变电极距离、电解温度、导电盐浓度以及电极电位与电解次序,考察了铅、钛电极溶解时电流密度与电流效率的变化;用红外、拉曼光谱等测试技术对纳米PbTiO3 前驱体进行了表征。结果表明,在c〔(Bu4N)Br〕=0 03mol/L的乙醇溶液中,保持电极距离0 8cm、电位12V、温度50℃电解钛片4h, 40℃电解铅片2h,每隔30min加入0 1mL乙酰丙酮,可制得铅、钛金属醇盐PbTi(OCH2CH3 )(6 y) (acac)y,前驱体中含有乙酰丙酮基团(acac- ),电流效率超过92%。

The relationship of electrode interval,potential,electrolysis temperature,and concentration of (Bu_4N)Br with current density and current efficiency in the course of dissolution of Pb and Ti anode was studied.IR and Raman spectroscopy were used to investigate the structure of the precursor of nano-sized PbTiO_3.The results showed that the precursor PbTi(OCH_2CH_3)_((6-y))(acac)_y was synthesized by electrochemical dissolution of titanium for 4h at 50 ℃ and then of lead for 2 h at 40 ℃ in ethanol solution of c〔(Bu_4N)Br〕=0.03 mol/L,into which 0.1 mL acetylacetone was added every 30 min The precursor contains acac-group.The current efficiency is over 92% when electrode interval is 0.8 cm and potential is 12 V.