Ni-P非晶态合金/酸化膨润土的制备及加氢性能

doi:10.16085/j.issn.1000-6613.2017.05.021

摘要/Abstract

摘要： 硝基苯液相催化加氢制苯胺是目前苯胺生产的一种重要方法，其中非晶态合金对该过程有较好的催化活性。本文采用微波加热干燥辅助浸渍-化学还原法制备了Ni-P非晶态合金/酸化膨润土催化剂，通过XRD、XPS、SEM、H₂-TPR、H₂-TPD对催化剂进行了表征，并用于硝基苯加氢制苯胺中，研究了催化剂结构与其催化加氢性能的关系。结果表明，微波加热法与传统加热法制备的催化剂均为非晶态结构，与传统干燥的方式相比，微波加热主要是提高了Ni活性位的分散度，改变了Ni活性位的表面电子态，增强了Ni活性中心与酸化膨润土载体之间的作用力。该催化剂的催化活性和稳定性显著高于由传统加热法制备的Ni-P非晶态合金/酸化膨润土。当Ni负载量为20% 时，在反应温度为110℃、氢气分压为1.8MPa的条件下，硝基苯的转化率和苯胺的选择性分别可达98.5%和98.8%，并且Ni-P非晶态合金/酸化膨润土催化剂循环使用6次后仍维持好的稳定性。

关键词: 非晶态合金, 膨润土, 微波辅助, 干燥, 硝基苯, 加氢, 稳定性

Abstract: Catalytic hydrogenation of nitrobenzene to aniline is an important method for preparation of aniline,for which amorphous alloy catalysts exhibit rather high activity. The Ni-P amorphous alloy/acid treated bentonite catalysts were prepared by using an impregnation-chemical reduction method assisted by microwave-drying,and characterized by XRD,XPS,SEM,H₂-TPR,and H₂-TPD. The prepared catalysts were then used for the catalytic hydrogenation of nitrobenzene to aniline to study the relationship between the catalysts' structure and their performance. The results showed that the Ni-P amorphous alloy/acid treated bentonite prepared by the two methods were both of amorphous structure. Compared with the traditional drying method,microwave-assisted drying method increased the dispersion of the Ni active sites,changed their surface electronic state,and improved the interactions between Ni and the acid-treated bentonite. The catalytic activity and the stability of the Ni-P/acid-treated bentonite catalysts dried by the microwave-assisted drying method were significantly higher than those dried by the traditional drying method. When the nickel loading amount was 20%,and at 110℃ with an initial H₂ pressure of 1.8MPa,the nitrobenzene conversion and the aniline selectivity over the Ni-P/acid treated bentonite amorphous alloy catalysts were 98.5% and 98.8%,respectively,which were still stable even after 6 recycles.

Key words: amorphous alloy, bentonite, microwave-assisted, drying, nitrobenzene, hydrogenation, stability

中图分类号:

徐云, 蒋月秀, 秦祖赠, 纪红兵. Ni-P非晶态合金/酸化膨润土的制备及加氢性能[J]. 化工进展, 2017, 36(05): 1719-1726.

XU Yun, JIANG Yuexiu, QIN Zuzeng, JI Hongbing. Preparation and hydrogenation property of Ni-P amorphous alloy/acid-treated bentonite catalysts[J]. Chemical Industry and Engineering Progress, 2017, 36(05): 1719-1726.

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