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

doi:10.11949/j.issn.0438-1157.20161014

Abstract

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（NO₃（₂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:

TQ032

LI Ying, LIU Xiaohong, AN Hualiang, ZHAO Xinqiang, WANG Yanji. Preparation of Ni/La-Al₂O₃ and its catalytic performance for one-pot sequential synthesis of 2-ethylhexanol from n-butyraldehyde[J]. CIESC Journal, 2017, 68(4): 1381-1389.

李颖, 刘肖红, 安华良, 赵新强, 王延吉. Ni/La-Al₂O₃的制备及催化正丁醛“一锅法”合成辛醇反应性能[J]. 化工学报, 2017, 68(4): 1381-1389.

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

Ni/La-Al₂O₃的制备及催化正丁醛“一锅法”合成辛醇反应性能

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