摘要
以2-氯吡啶为起始原料,在冰醋酸介质中用质量分数为30%H2O2直接氧化,再与NaSH进行巯基化,然后同ZnSO4螯合成盐得到吡啶硫酮锌(ZPT)。同时还研究了溶剂的回收套用、不同催化剂对氧化反应的影响及不同pH值对巯基化反应的影响,优化条件下ZPT总收率可达78 0%。通过对溶剂的循环使用,减少了溶剂(冰醋酸)用量66 7%,反应收率也提高了10%左右,巯基化反应的pH值控制在9～10。产品经熔点、含量、pH值和IR的测试,达到了出口标准的要求。
N-oxide-2-mercaptopyridine zinc salt was synthesized from 2-chloropyridine through oxidation with 30 %(mol)H2O2 in glacial acetic acid,mercapto-reaction with NaSH and chelation with ZnSO4.The influences of recycle of solvent,various catalysts on oxidation and influence of pH on mercapto-reaction,were investigated.The total yield of ZPT under optimum conditions is 780 %.Using solvent recycle way,the consumption of solvent(HAc) is decreased by 667 %.Yield could be increased by 10 %,pH value of mercapto-reaction is 9～10.The product quality indices on melting point,purity,pH value and IR spectrograpy,meet the standard specifications acceptable for international market.
出处
《日用化学工业》
CAS
CSCD
北大核心
2003年第5期340-342,共3页
China Surfactant Detergent & Cosmetics
