摘要
以Ti基PbO2 为阳极 ,Cu或Ni为阴极 ,在硫酸介质中 ,电解氧化 4 甲基吡啶合成了异烟酸。经过实验确定的最佳合成条件为 :c(硫酸 ) =4 6 0mol/L ,c(4 甲基吡啶 ) =0 6 0mol/L ,电解电流密度i=6 0mA/cm2 ,t=6 0℃。在此条件下 ,异烟酸的收率为 6 4 6 % ,电流效率为 6 7%。同时还研究了电解过程中反应物转化率、电流效率、槽压的变化规律。经示波极谱、红外光谱和熔点测定法证明电合成的物质为异烟酸 ,质量分数为 97 7%。
Isonicotinic acid(4-picolinic acid) was synthesized from 4-methylpyridine using electrochemical method in sulfuric acid solution with Ti/PbO2 as anode and Cu or Ni as cathode in an H-shaped electrolytic cell separated by a cation exchange membrane.The appropriate reaction conditions obtained were as follows.The H2SO4 concentration was 4.60 mol/L,the 4-methylpyridine concentration was 0.60 mol/L,the electrolytic current density was 60 mA/cm2 and the temperature was 60 ℃.The yield of 4-picolinic acid was 64.6% and the current efficiency could be 67% under these conditions.The relationships among yield,current efficiency,bath voltage and electrolysis time were studied.The product was identified by oscillopolarography,infrared spectrometry and melting point test.The purity of 4-picolinic acid determined by oscillopolarography was about 97.7%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2000年第z1期78-81,共4页
Fine Chemicals
关键词
异烟酸
4-甲基吡啶
钛基二氧化铅电极
电化学合成
示波极谱法
isonicotinic acid
4-methylpyridine
titanium electrode coated with lead dioxide
electrochemical synthesis
oscillopolarography
