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2,6-二叔丁基-4-亚硝基苯酚的合成及表征
引用本文:李卫平,刘茵,张鹏云,霍利春,张伟,杨文龙.2,6-二叔丁基-4-亚硝基苯酚的合成及表征[J].陕西化工,2012(9):1575-1578.
作者姓名:李卫平  刘茵  张鹏云  霍利春  张伟  杨文龙
作者单位:[1]甘肃省化工研究院,甘肃兰州730000 [2]西北师范大学化学化工学院,甘肃兰州730070
摘    要:以2,6-二叔丁基苯酚、浓硫酸及亚硝酸钠为原料,在乙醇中合成了抗氧剂中间体2,6-二叔丁基-4-亚硝基苯酚,考察了溶剂种类、反应温度、反应时间、投料比和投料次序对反应的影响。结果表明,最佳工艺条件为:乙醇为溶剂,反应温度25℃,n(2,6-二叔丁基苯酚)∶n(浓硫酸)∶n(亚硝酸钠)=1∶1.1∶1.1,投料次序为先滴加浓硫酸,再滴加亚硝酸钠溶液,反应时间为2 h。在该条件下,产物重结晶收率为92.0%,产物色谱纯度≥99.7%。

关 键 词:2  6-二叔丁基苯酚  2  6-二叔丁基-4-亚硝基苯酚  亚硝化  抗氧剂

Synthesis and characterization of 2,6-di-tert-butyl-4-nitrosophenol
LI Wei-ping,LIU Yin,ZHANG Peng-yun,HUO Li-chun,ZHANG Wei,YANG Wen-long.Synthesis and characterization of 2,6-di-tert-butyl-4-nitrosophenol[J].Applied Chemical Industry,2012(9):1575-1578.
Authors:LI Wei-ping  LIU Yin  ZHANG Peng-yun  HUO Li-chun  ZHANG Wei  YANG Wen-long
Affiliation:1. Gansu Insititute of Chemical Industry, Lanzhou 730000 ,China;2. College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070, China)
Abstract:The antioxidant intermediate compound 2,6-di-tert-butyl-4-nitrosophenol was synthesized, the reaction of 2,6-di-tert-butylphenol with concentration sulfuric acid and sodium nitrite as raw materials. The effects of the type of solvent, reaction temperature, reaction time, mole ratio of materials, and feeding sequence was investigated respectively. The results showed that the optimum process conditions with the yield of 92.0% and purity of 99.7 % : ethanol as solvent, reaction temperature 25 ℃, n ( 2,6-di-tert-butyl- phenol) : n( concentration sulfuric acid): n(sodium nitrite) = 1: 1. 1:1.1, the reaction system of concen- tration sulfuric acid and phenol was added dropwise of the solution of sodium nitrite,reaction time 2 h.
Keywords:2  6-di-tert-butylphenol  2  6-di-tert-butyl-4-nitrosophenol  nitrosation  antioxidant
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