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[1]熊曼,黄磊,刘晓云,等.铑催化的还原胺化合成一级胺[J].南京工业大学学报(自然科学版),2014,36(04):13-17.[doi:10.3969/j.issn.1671-7627.2014.04.003]
 XIONG Man,HUANG Lei,LIU Xiaoyun,et al.Rhodium catalyzed reductive amination of aldehydes to primary amines with ammonium acetate[J].Journal of NANJING TECH UNIVERSITY(NATURAL SCIENCE EDITION),2014,36(04):13-17.[doi:10.3969/j.issn.1671-7627.2014.04.003]
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铑催化的还原胺化合成一级胺()
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《南京工业大学学报(自然科学版)》[ISSN:1671-7627/CN:32-1670/N]

卷:
36
期数:
2014年04期
页码:
13-17
栏目:
出版日期:
2014-07-01

文章信息/Info

Title:
Rhodium catalyzed reductive amination of aldehydes to primary amines with ammonium acetate
文章编号:
1671-7627(2014)04-0013-05
作者:
熊曼黄磊刘晓云席其周黄军
南京工业大学 化学化工学院 材料化学工程国家重点实验室,江苏 南京 210009
Author(s):
XIONG ManHUANG LeiLIU XiaoyunXI QizhouHUANG Jun
State Key Laboratory of Material-Oriented Chemical Engineering,College of Chemistry and Chemical Engineering,Nanjing Tech University,Nanjing 210009,China
关键词:
还原胺化 一级胺 苯甲醛 乙酸铵
Keywords:
rhodium reductive amination primary amines benzaldehyde ammonium acetate
分类号:
TQ032.4
DOI:
10.3969/j.issn.1671-7627.2014.04.003
文献标志码:
A
摘要:
采用浸渍法制备Rh/CeO2催化剂。通过粉末X线衍射仪(XRD)、N2吸附-脱附分析、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等对催化剂的性能进行表征。以苯甲醛和乙酸铵的还原胺化反应为模板反应,考察Rh/CeO2催化剂的催化性能。结果表明:Rh/CeO2催化剂具有多孔结构,且其在醛的还原胺化反应中表现出较高的活性和选择性。在反应温度为50 ℃、H2压力为0.1 MPa、乙醇作溶剂、n(乙酸铵):n(苯甲醛):n(Rh/CeO2)=50:10:0.1时,苯甲醛的转化率为100%,苄胺的产率为88%。催化剂重复使用5次后,依旧可以保持较高的催化活性。在优化条件下,系列苯甲醛均可选择性地还原胺化得到相应一级胺。
Abstract:
The rhodium catalyst Rh/CeO2 was prepared by incipient wetness impregnation method.The sample was characterized by X-ray powder diffraction(XRD),N2 adsorption-desorption analysis,scanning electron microscope(SEM), and transmission electron microscope(TEM).The Rh/CeO2 catalysed reductive amination of benzaldehyde with ammonium acetate was investigatied as a model reaction.Results showed that Rh/CeO2 had a porous structure and was highly active for the reductive amination of benzaldehyde.The conversion of benzaldehyde and the yield to benzylamine were 100% and 88% under the optimized operation conditions at 50 ℃,in ethanol,at 0.1 MPa H2,with the ratio of starting substances as n(NH4OAC):n(benzaldehyde):n(Rh/CeO2)=50:10:0.1.The Rh/CeO2 catalyst was reusable and active after 5 times recycles.Several aldehydes were used for the reductive amination,and most of the primary amines were obtained in high yields.

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备注/Memo

备注/Memo:
收稿日期:2013-08-02
基金项目:国家自然科学基金(21136005, 21125629); 国家高技术研究发展计划(863计划)(2012AA03A606)
作者简介:熊曼(1988—),女,江苏徐州人,硕士,主要研究方向为有机工业催化; 黄军(联系人),教授,E-mail:junhuang@njtech.edu.cn..
更新日期/Last Update: 2014-07-31