CIESC Journal ›› 2017, Vol. 68 ›› Issue (4): 1381-1389.DOI: 10.11949/j.issn.0438-1157.20161014

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Preparation of Ni/La-Al2O3 and its catalytic performance for one-pot sequential synthesis of 2-ethylhexanol from n-butyraldehyde

LI Ying, LIU Xiaohong, AN Hualiang, ZHAO Xinqiang, WANG Yanji   

  1. Hebei Provincial Key Laboratory of Green Chemical Technology and Efficient Energy Saving, School of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130, China
  • Received:2016-07-20 Revised:2017-01-16 Online:2017-04-05 Published:2017-04-05
  • Supported by:

    supported by the National Natural Science Foundation of China (21476058, 21506046, 21236001).

Ni/La-Al2O3的制备及催化正丁醛“一锅法”合成辛醇反应性能

李颖, 刘肖红, 安华良, 赵新强, 王延吉   

  1. 河北工业大学化工学院, 绿色化工与高效节能河北省重点实验室, 天津 300130
  • 通讯作者: 赵新强
  • 基金资助:

    国家自然科学基金项目(21476058,21506046,21236001)。

Abstract:

2-Ethylhexanol (2EHO), an important organic chemical compound, is commercially produced by the following three steps:propylene hydroformylation to n-butyraldehyde, n-butyraldehyde self-condensation to 2-ethyl-2-hexenal (2E2H), and 2E2H hydrogenation to 2EHO. One-pot synthesis of 2EHO was studied by sequential n-butyraldehyde aldol condensation and hydrogenation reaction with synthesized Ni/La-Al2O3 catalyst. The investigation of preparation conditions of Ni/La-Al2O3 on its catalytic performance showed that most suitable preparation condition for Ni/La-Al2O3 was Ni loading of 25% (mass), after immersion at Ni(NO3)2 and aging, then 4 h at calcination temperature of 500℃, and finally 3 h at reduction temperature of 550℃. Under the optimal reaction conditions, the catalyst could achieve 100% n-butyraldehyde conversion and 67.0% yield of 2EHO. Combined with results of XRD and SEM analyses, γ-Al2O3 hydration was one of the main reasons for the deactivation of Ni/La-Al2O3.

Key words: n-butyraldehyde, catalyst, one-pot synthesis, hydrogenation, integration

摘要:

辛醇(2-乙基己醇)是重要的基本有机化工原料,其工业生产由丙烯氢甲酰化合成正丁醛、正丁醛自缩合制备2-乙基-2-己烯醛(辛烯醛)、辛烯醛加氢生成辛醇3个反应单元构成。本研究旨在以Ni/La-Al2O3为催化剂实现正丁醛顺序自缩合和加氢“一锅法”合成辛醇。首先制备了Ni/La-Al2O3催化剂,并考察了制备条件对其催化性能的影响,结果表明Ni/La-Al2O3适宜的制备条件为Ni负载量为25%(质量分数),浸渍Ni(NO32并老化后,于500℃下焙烧4 h,再于550℃还原3 h。在适宜的反应条件下,正丁醛完全转化,辛醇的收率为67.0%。结合XRD和SEM表征发现,γ-Al2O3水合是导致Ni/La-Al2O3催化剂失活的主要原因之一。

关键词: 正丁醛, 催化剂, 一锅法合成, 加氢, 集成

CLC Number: