SrHPO_4/BaHPO_4催化合成2-甲基三乙烯二胺及其类似物  

THE CATALYTIC SYNTHESIS OF 2-METHYL-1,4-DIAZABICYCLO[2.2.2]OCTANE AND ITS ANALOGUES ON SrHPO_4/BaHPO_4

作　　者：黄朋勉[1] 易霞[1] 陈金星 周智慧[1] 王梓鉴 周胜 Huang Pengmian;Yi Xia;Chen Jinxin;Zhou Zhihui;Wang Zijian;Zhou Sheng(School of Chemistry and Bioengineering, Changsha University of Science and Technology, Changsha 410114, Hu＇nan,China)

机构地区：[1]长沙理工大学化学与生物工程学院,湖南长沙410114

出　　处：《精细石油化工》2018年第3期11-14,共4页Speciality Petrochemicals

摘　　要：以2-甲基哌嗪及其类似物和2-氯乙醇为原料,采用气固相催化工艺,以SrHPO_4/BaHPO_4为催化剂,两步反应合成高收率、高纯度的2-甲基三乙烯二胺及其类似物,并考察了两步反应条件对目标产物产率的影响。较佳的合成条件为:第一步反应,n(2-甲基哌嗪及其类似物)∶n(2-氯乙醇)=1.0∶2.0,反应温度70℃,反应时间6h;第二步反应,预热器温度200℃,固定床反应温度340℃,进料量2mL/min。2-甲基三乙烯二胺的两步反应产物收率84%,纯度98%以上;三乙烯二胺的两步反应收率88%,纯度98%以上。2-Methyl-1,4-diazabicyclo[2.2.2]octane and its analogues with high yield and purity were synthesized from 2-methyl piperazine with its analogues and 2-chloroethanol in fixed bed with SrHPO4/BaHPO4 as the catalyst.The influence of two-step reaction conditions on the yield and content of products was studied.The reaction conditions of first step are that the optimal ratio between 2-methyl piperazine with its analogues and 2-chloroethanol was 1.0∶2.0 at 70 ℃ and reaction time was 6 h.The reaction conditions of second step are that the preheater temperature was 200℃and optimal temperature of fixed bed was 340 ℃ with feed rate 2 mL/min.The total yield of 2-methyl-1,4-diazabicyclo[2.2.2]octane was 84% with the purity over 98% and the total yield of 1,4-diazabicyclo[2.2.2]octane was 88% with the purity over 98%.

关 键 词：2-甲基三乙烯二胺 三乙烯二胺 磷酸氢锶/磷酸氢钡 固定床 

分 类 号：TQ226.3[化学工程—有机化工]