Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-(3-nitro-4-methoxyphenyl) Acetamide

doi:10.1016/S1004-9541(13)60497-8

Chin.J.Chem.Eng. ›› 2013, Vol. 21 ›› Issue (6): 622-626.DOI: 10.1016/S1004-9541(13)60497-8

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Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-(3-nitro-4-methoxyphenyl) Acetamide

ZHANG Qunfeng, LÜ Jinghui, MA Lei, LU Chunshan, LIU Wei, LI Xiaonian

Industrial Catalysis Institute, State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology, Zhejiang University of Technology, Hangzhou 310032, China

Received:2012-12-13 Revised:2013-03-09 Online:2013-07-03 Published:2013-06-28
Contact: LI Xiaonian
Supported by:
Supported by the Natural Science Foundation of Zhejiang Provincial (LY12B03009) and Program for Zhejiang Leading Team of Science and Technology Innovation (2011R09020-03).

Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-(3-nitro-4-methoxyphenyl) Acetamide

张群峰, 吕井辉, 马磊, 卢春山, 刘维, 李小年

Industrial Catalysis Institute, State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology, Zhejiang University of Technology, Hangzhou 310032, China

通讯作者: LI Xiaonian
基金资助:
Supported by the Natural Science Foundation of Zhejiang Provincial (LY12B03009) and Program for Zhejiang Leading Team of Science and Technology Innovation (2011R09020-03).

Abstract

Abstract: Deactivation of Pd/C catalyst often occurs in liquid hydrogenation using industrial materials. For instance, the Pd/C catalyst is deactivated severely in the hydrogenation of N-(3-nitro-4-methoxyphenyl) acetamide. In this study, the chemisorption of sulfur on the surface of deactivated Pd/C was detected by energy dispersive spectrometer and X-ray photoelectron spectroscopy. Sulfur compounds poison the Pd/C catalyst and increase the formation of azo deposit, reducing the activity of catalyst. We report a mild method to regenerate the Pd/C catalyst: wash the deposit by N,N-dimethylformamide and oxidize the chemisorbed sulfur by hot air. The regenerated Pd/C catalyst can be reused at least ten runs with stable activity.

Key words: Pd/C catalyst, hydrogenation, deactivation, regeneration, sulfur

摘要： Deactivation of Pd/C catalyst often occurs in liquid hydrogenation using industrial materials. For instance, the Pd/C catalyst is deactivated severely in the hydrogenation of N-(3-nitro-4-methoxyphenyl) acetamide. In this study, the chemisorption of sulfur on the surface of deactivated Pd/C was detected by energy dispersive spectrometer and X-ray photoelectron spectroscopy. Sulfur compounds poison the Pd/C catalyst and increase the formation of azo deposit, reducing the activity of catalyst. We report a mild method to regenerate the Pd/C catalyst: wash the deposit by N,N-dimethylformamide and oxidize the chemisorbed sulfur by hot air. The regenerated Pd/C catalyst can be reused at least ten runs with stable activity.

关键词: Pd/C catalyst, hydrogenation, deactivation, regeneration, sulfur

ZHANG Qunfeng, LÜ Jinghui, MA Lei, LU Chunshan, LIU Wei, LI Xiaonian . Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-(3-nitro-4-methoxyphenyl) Acetamide[J]. Chin.J.Chem.Eng., 2013, 21(6): 622-626.

张群峰, 吕井辉, 马磊, 卢春山, 刘维, 李小年. Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-(3-nitro-4-methoxyphenyl) Acetamide[J]. Chinese Journal of Chemical Engineering, 2013, 21(6): 622-626.

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Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-(3-nitro-4-methoxyphenyl) Acetamide

Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-(3-nitro-4-methoxyphenyl) Acetamide

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