Li Zuo, Qiao Qing-dong
2001
Citations
0
Influential Citations
5
Citations
Journal
Journal of Petrochemical Universities
Abstract
The isoniacin (4-picolinic acid) was electrochemically synthesized from 4-methypyridine in 25% sulfuric acid aqueous solution using Ti/PbO 2 as anode and Cu or Ni as cathode in the H shape electrolysis cell that was separated by cation exchange membrane. The appropriate synthesis conditions obtained by experiment were that the mass fraction of the H 2SO 4 was 25%, the 4-methylpyridine concentration was 0.60 mol/L, the electrolytic current density was 60 mA/cm 2 and the temperature was 60 ℃. The conversion of 4-methylpyidine and the current efficiency could be 64.6% and 67% respectively in such conditions. The relationships among conversion, current efficiency and bath voltage with electrodes, current density, temperature and electrolysis time were studied. In addition, the 4-picoline acid in sulfuric acid solution could yield a stable electrochemical reduction peak at -0.72 V versus SCE, for this reason the oscillopolarographic method to determine isoniacin was proposed. The product was identified by oscillopolarography, infrared spectrometry and melting point test. The purity of 4-picolinic acid determined by the oscillopolarography was about 97.7%.