N,N′-二环己基二氮烯-N,N′-二氧化物的合成  

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

作　　者：张珍明 夏天 黄文静 彭晓含 陈达 李树安 ZHANG Zhen-ming;XIA Tian;HUANG Wen-jing;PENG Xiao-han;CHEN Da;LI Shu-an(School of Chemical Engineering & Technology, Jiangsu Ocean University, Lianyungang 222005, China)

机构地区：[1]江苏海洋大学化学工程学院,江苏连云港222005

出　　处：《兰州理工大学学报》2021年第1期78-82,共5页Journal of Lanzhou University of Technology

基　　金：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)。

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(H_(2)O_(2))∶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、^(1)H NMR、^(13)C NMR和MS表征了产物的结构.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,^(1)H NMR,^(13)C NMR and MS.

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 

分 类 号：TQ396[化学工程]