兰州理工大学学报

兰州理工大学学报 ›› 2021, Vol. 47 ›› Issue (1): 78-82.

• 化工与轻工 • 上一篇    下一篇

N,N'-二环己基二氮烯-N,N'-二氧化物的合成

张珍明, 夏天, 黄文静, 彭晓含, 陈达, 李树安   

  1. 江苏海洋大学 化学工程学院, 江苏 连云港 222005
  • 收稿日期:2020-03-25 出版日期:2021-02-28 发布日期:2021-03-11
  • 作者简介:张珍明(1964-),女,山东烟台人,博士,教授.
  • 基金资助:
    江苏省优势学科建设工程项目(5511201901X),江苏省大学生创新项目(SD201911641104003),江苏省苏北科技专项(SZ-LYG202017),连云港市“花果山英才计划”科技副总项目(2019.12)

Synthesis of N,N'-dicyclohexyl-diazen-N,N'-dioxide

ZHANG Zhen-ming, XIA Tian, HUANG Wen-jing, PENG Xiao-han, CHEN Da, LI Shu-an   

  1. School of Chemical Engineering & Technology, Jiangsu Ocean University, Lianyungang 222005, China
  • Received:2020-03-25 Online:2021-02-28 Published:2021-03-11

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摘要： 研究了用组合氧化剂过碳酸钠-过氧化氢-四乙酰乙二胺氧化环己胺制备N,N'-二环己基二氮烯-N,N'-二氧化物,通过正交实验、单因素实验考察了氧化剂各成分投料比、pH、反应温度、反应时间及反应后陈化时间对产物收率的影响.优化的工艺条件为n(环己胺):n(过碳酸钠):n(H2O2):n(四乙酰乙二胺)=1.0:3.0:3.0: 1.75,pH=9,在水/乙酸乙酯混合溶液(物质的量的比为5.3:1.0)中33 ℃下反应3 h,陈化12 h,收率98.3%.用IR、1H NMR、13C NMR和MS表征了产物的结构.

关键词: N,N'-二环己基二氮烯-N, N'-二氧化物, 环己胺, 过碳酸钠, 过氧化氢, 四乙酰乙二胺, 氧化

Abstract: N,N'-dicyclohexyldiazene-N,N'-dioxide was prepared by oxidation of cyclohexylamine with the combined oxidant of sodium percarbonate-hydrogen peroxide-tetraacetylethylenediamine. Effects of the ratio of oxidant, pH, reaction temperature, reaction time and aging time after reaction on the yield were investigated by either orthogonal or single-factor experiments. The optimized process conditions are as follows: n(cyclohexylamine): n(sodium percarbonate): n(hydrogen peroxide): n(tetraacetylethylenediamine)=1:3.0:3.0:1.75, in water/ethyl acetate mixed solution (rotio of amount of substance=5.3:1.0) with pH =9 at 33 ℃ reaction for 3 h, and aging for 12 h, the yield reaches as high as 98.3%. The structure of the product was characterized by IR, 1H NMR, 13C NMR and MS.

Key words: N,N'-dicyclohexyl-diazen-N, N'-dioxide, cyclohexylamine, sodium percarbonate, hydrogen peroxide, tetraacetylethylenediamine, oxidation

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