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浙江大学学报(工学版)
J4  2010, Vol. 44 Issue (12): 2401-2405    DOI: 10.3785/j.issn.1008-973X.2010.12.028
化学工程     
固定床催化合成N,N,N′,N′-四甲基乙二胺的研究
张涛1, 陈汉庚1, 张旭1, 韦隆武2, 钱超1, 陈新志1
1.化学工程联合国家重点实验室,浙江大学化学工程与生物工程学系,浙江 杭州 310027；
2.宁波永顺精细化工有限公司,浙江 宁波 315204
Catalytic synthesis of N,N,N′,N′-tetramethylethylenediamine
in fixed-bed reactor
ZHANG Tao1, CHEN Han-geng1, ZHANG Xu1, WEI Long-wu2,
QIAN Chao1, CHEN Xin-zhi1
1. State Key Laboratory of Chemical Engineering, Department of Chemical and Biological Engineering, Zhejiang
University, Hangzhou 310027, China； 2. Ninbo Yongshun Fine Chemical Co.Ltd., Ningbo 315204, China
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摘要：

通过自制备的金属负载型催化剂,以二甲胺和乙二醇为原料,在气固固定床反应器中合成了N,N,N′,N′-四甲基乙二胺.以γ-Al2O3为载体,Cu、Ni、Cr、Zn等金属为活性组分,通过浸渍法制备了3种二元金属负载型催化剂：Cu-Ni型、Cu-Zn型、Cu-Cr型.在相同条件下对3种催化剂的催化性能进行了考察,对乙二醇转化率及四甲基乙二胺的选择性进行了分析,结果表明：Cu-Ni型催化剂的催化效果最佳.通过平行实验对反应温度、胺醇的物质的量比及体积空速进行了研究,获得了较优的条件区间范围.根据平行实验结果,采用响应面实验设计方法（Design Expert软件）对反应条件进行了优化,获得了最优的反应条件：以Cu-Ni为活性组分的催化剂进行催化,反应温度为204.81 ℃,胺醇的物质的量比为5.27,体积空速为0.29 h-1,最佳产率可以达到79.84%.
Abstract:

N,N,N′,N′-tetramethylethylenediamine was obtained by dehydration of dimethyl amine and glycol in a fixed-bed reactor under the selfmade supported metal catalysts. First, three types of catalysts (Cu-Ni, Cu-Cr, Cu-Zn) were prepared through impregnation method with γ-Al2O3 as the carrier and Cu, Ni, Cr, Zn as the active components. The performance of these catalysts, which was evaluated by the conversion of glycol and the selectivity of tetramethylethylenediamine, was investigated under the same condition. The results indicated the best performance of Cu-Ni type. A series of parallel experiments were carried out to find out the appropriate range of temperature, the molar ratio of ethyl diamine/glycol and volume velocities. The experimental conditions were eventually optimized by response surface methodology (Design Expert) and the optimal values were: 204.81 ℃, molar ratio of ethyl diamine/glycol of 5.27, velocity of 0.29 h-1, with the highest yield of 79.84%.
出版日期: 2010-12-01
:  TQ 032.41  
基金资助:

国家自然科学基金资助项目(20776127)；浙江省科技计划资助项目(2008C010061)；宁波市科技计划资助项目(2010B10009).
通讯作者: 陈新志,男,教授,博导.     E-mail: xzchen@zju.edu.cn
作者简介: 张涛（1984—）,男,河北廊坊人,硕士生,从事有机医药中间体研究.
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引用本文:

张涛, 陈汉庚, 张旭, 韦隆武, 钱超, 陈新志. 固定床催化合成N,N,N′,N′-四甲基乙二胺的研究[J]. J4, 2010, 44(12): 2401-2405.

ZHANG Tao, CHEN Han-geng, ZHANG Xu, WEI Long-wu,QIAN Chao, CHEN Xin-zhi. Catalytic synthesis of N,N,N′,N′-tetramethylethylenediamine
in fixed-bed reactor. J4, 2010, 44(12): 2401-2405.

链接本文:

http://www.zjujournals.com/eng/CN/10.3785/j.issn.1008-973X.2010.12.028    或    http://www.zjujournals.com/eng/CN/Y2010/V44/I12/2401

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