文章摘要
冯柏成,初晓东,董静静,金岩.电氧化合成Co3+及其在对甲砜基苯甲酸制备中的应用[J].精细化工,2019,36(11):
电氧化合成Co3+及其在对甲砜基苯甲酸制备中的应用
Electrooxidation synthesis of Co3+ and its application in the preparation of p-formylbenzoic acid
投稿时间:2018-12-24  修订日期:2019-04-25
DOI:
中文关键词: 电氧化  对甲砜基苯甲酸  绿色化工
英文关键词: Electrooxidation  P-methyl sulfone benzoic acid  Green chemical industry
基金项目:
作者单位E-mail
冯柏成 青岛科技大学 fbc515@163.com 
初晓东 青岛科技大学  
董静静 青岛科技大学  
金岩 青岛科技大学 qaz309@126.com 
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中文摘要:
      本文对Co3+的电氧化合成以及用作氧化对甲砜基甲苯合成对甲砜基苯甲酸进行了系统研究。研究表明,选用阳极二氧化铅、阴极铅为电极板,陶瓷膜作为阳离子交换膜,电解液浓度为C(Co2+)=0.5mol/L、C(硫酸)=4.0mol/L、C(硫酸铵)=0.15mol/L,电极间距d=2cm、电流密度J=350A/m2、电解温度t=10℃,电解液Co2+转化率可达80%,电解氧化电流效率67.5%。在进行对甲砜基甲苯的氧化时,控制电解液浓度为C(Co3+)=0.4mol/L、C(硫酸)=4.0mol/L、C(硫酸铵)=0.15mol/L,Co3+与对甲砜基甲苯的摩尔比n(Co3+):n(对甲砜基甲苯)=6:1,反应温度30℃,反应时间30min,对甲砜基苯甲酸的收率可达97.8%,精制后纯度在98.5%以上。
英文摘要:
      In this paper, the synthesis of Co3+ by electrooxidation and the synthesis of P-methyl sulfone benzoic acid by oxidation of P-methyl sulfone toluene were systematically studied.Studies have shown that lead dioxide anode, cathode lead electrode plates, ceramic membrane as a cation exchange membrane and electrolyte concentration to C(Co2+)=0.5 mol/L, C(sulfuric acid)=4.0 mol/L, C(ammonium sulfate)=0.15 mol/L, electrode spacing d=2cm, the current density J=350 A/m2, electrolytic temperature t=10 ℃, the electrolyte Co2+ conversion rate could reach 80% and the electrolytic oxidation current efficiency was 67.5%.In the matrix oxidation process, the concentration of electrolyte C(Co3+)=0.4mol/L, C(sulfuric acid)=4.0 mol/L,C(ammonium sulfate)=0.15 mol/L, the mole ratio of Co3+ and thiamphenicol toluene 6:1, reaction temperature 30 ℃ and reaction time 30min, the yield of benzoic acid thiamphenicol could reach 97.8% and purity was 99% after refining.
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