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Preparation method for synthesizing aniline catalyst by undergoing hydrogenation reaction on nitrobenzene

A technology of hydrogenation reaction and catalyst, which is applied in the field of preparation of aniline catalyst for hydrogenation reaction of nitrobenzene, can solve problems such as difficulties in batch preparation, and achieve the effects of cheap and easy-to-obtain raw materials, mild reaction conditions, and easy industrialization

Inactive Publication Date: 2012-07-11
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is kind of quick and gentle, but very difficult to make in batches

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The steps of preparing Pd-carbon nanotube catalyst: first, PdCl 2 Trisodium citrate was added to the aqueous solution so that the molar ratio of trisodium citrate to Pd was 3.0, and deionized water was added and stirred. Add NaBH 4 solution, the color of the solution turns brownish black, indicating that the Pd nanoparticles have been reduced. This solution is designated as solution I.

[0025] Secondly, the multi-walled carbon nanotubes were added into deionized water and ultrasonically treated for 10 min to obtain suspension II. Mix solution I and suspension II at room temperature, stir for 10 h, filter, wash with deionized water three times, and dry in vacuum at 60°C for 6 h. The obtained Pd-carbon nanotube catalyst has a Pd loading of 5 wt%.

[0026] Electron microscopy photos of Pd-carbon nanotube catalysts show that Pd nanoparticles are evenly dispersed on the surface of multi-walled carbon nanotubes, with almost no agglomeration. The size of Pd nanoparticles ...

Embodiment 2

[0028] PdCl 2 Trisodium citrate was added to the aqueous solution so that the molar ratio of trisodium citrate to Pd was 0.8, and deionized water was added and stirred. Add NaBH 4 solution, the color of the solution turns brownish black, indicating that the Pd nanoparticles have been reduced. This solution is designated as solution I.

[0029] Secondly, the multi-walled carbon nanotubes were added into deionized water and ultrasonically treated for 10 min to obtain suspension II. Mix solution I and suspension II at room temperature, stir for 10 h, filter, wash with deionized water three times, and dry in vacuum at 60°C for 6 h. The obtained Pd-carbon nanotube catalyst has a Pd loading of 10 wt%. Electron micrographs of Pd-carbon nanotube catalysts showed that Pd NPs were uniformly dispersed on the outer wall of MWCNTs, and the particle size was about 6.0nm. The peak near 40° in the XRD pattern of the catalyst is the (111) crystal plane of metal Pd nanoparticles, and the p...

Embodiment 3

[0031] PdCl 2 Trisodium citrate was added to the aqueous solution so that the molar ratio of trisodium citrate to Pd was 5.0, and deionized water was added and stirred. Add NaBH 4 solution, the color of the solution turns brownish black, indicating that the Pd nanoparticles have been reduced. This solution is designated as solution A.

[0032] Secondly, the multi-walled carbon nanotubes were added into deionized water and ultrasonically treated for 10 min to obtain suspension II. Mix solution I and suspension II at room temperature, stir for 10 h, filter, wash with deionized water three times, and dry in vacuum at 60°C for 6 h. The obtained Pd-carbon nanotube catalyst has a Pd loading of 5 wt%. The Pd-carbon nanotube catalyst has an average particle size of 3.0nm.

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Abstract

The invention discloses a preparation method for synthesizing an aniline catalyst by undergoing a hydrogenation reaction on nitrobenzene. The method comprises the following steps of: reducing a PdCl2 aqueous solution under the protection of sodium citrate by taking a NaBH4 aqueous solution as a reducing agent to obtain Pd nanoparticle sol; and mixing and stirring an ultrasonically-treated carbon nanotube in the aqueous solution with the Pd nanoparticle sol to form a Pd-carbon nanotube catalyst. The aniline catalyst shows very high activity in a reaction for synthesizing aniline through hydrogenation of nitrobenzene, and has long cycle life.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for synthesizing aniline by hydrogenation reaction of nitrobenzene. Background technique [0002] Due to physical effects such as surface effect, small size effect, quantum size effect and macroscopic quantum tunneling effect, metal nanoparticles have unique optical, electrical, mechanical and other excellent properties, and have broad application prospects in the high-tech field. Highly dispersed Pt, Pd, Ni, Rh, etc. have been reported (Catal.Commun., 2009(10): 1203-1206.Catal.Lett., 2002(84): 205-208.Mater.Chem.Phys., 2007 (103):225-229.) can be applied in heterogeneous hydrogenation reactions, and exhibit very high activity and selectivity. However, due to the relatively large specific surface energy of metal nanoparticles, they are easy to agglomerate, resulting in reduced catalyst activity and lifetime. Carbon nanotubes have a very large specific surface area, good electrical conductivi...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J21/18B01J37/34B01J37/00B01J35/02C07C211/46C07C209/36
Inventor 王晓来刘华陈龙
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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