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Prepn of nanometer carbon material supported metal catalyst for hydrogenating chloronitrobenzene to synthesize chloroaniline

A technology of chloronitrobenzene and chloroaniline, which is applied in the field of catalysts for the synthesis of chloroaniline by hydrogenation of chloronitrobenzene, which can solve the problems of poor dispersion of catalyst active components, uneven metal particle size, and catalyst agglomeration and other problems, to achieve the effect of excellent reaction performance, short preparation cycle and low dechlorination performance

Inactive Publication Date: 2007-08-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The preparation of supported catalysts usually adopts the traditional impregnation method. The preparation process is simple and easy to operate. However, the active components of the prepared catalysts have poor dispersion and the metal particles are not uniform in size, resulting in low activity.
Due to the weak interaction between the carbon support and the metal, the catalyst prepared by the impregnation method usually has a very serious agglomeration phenomenon

Method used

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  • Prepn of nanometer carbon material supported metal catalyst for hydrogenating chloronitrobenzene to synthesize chloroaniline
  • Prepn of nanometer carbon material supported metal catalyst for hydrogenating chloronitrobenzene to synthesize chloroaniline
  • Prepn of nanometer carbon material supported metal catalyst for hydrogenating chloronitrobenzene to synthesize chloroaniline

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Experimental program
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Effect test

Embodiment 1

[0016] (1) Carbon nanofiber or carbon nanotube activation treatment:

[0017] Put carbon nanofibers or carbon nanotubes into a round bottom flask, add a mixed solution of sulfuric acid and nitric acid with a volume ratio of 3:1, reflux at 120°C for 4 hours, filter, wash with water until the filtrate is neutral, and dry in air at 100°C for 12 Hour.

[0018] (2 Preparation of carbon nanofiber supported metal nickel catalyst

[0019] Weigh 0.212g Ni(AC) 2 Add 0.5g mixed acid-treated carbon nanofibers into 50mL ethylene glycol, ultrasonically disperse for 5 minutes, then raise the temperature to 80°C, add 0.9mL 0.2M Na 2 CO 3 The aqueous solution was filtered after constant temperature for 1 hour, washed with water, and dried to obtain the catalyst precursor. Put the obtained precursor in a tubular heating furnace, raise the temperature to 400°C at a rate of 3°C / min in a high-purity nitrogen atmosphere, keep it warm for 4 hours, then switch to a mixed gas of nitrogen and hydro...

Embodiment 2

[0023] (1) The carbon nanofiber activation treatment is the same as in Example 1.

[0024] (2) Preparation of carbon nanofiber-supported metal nickel catalyst

[0025] Weigh 0.212g Ni(AC) 2 Add 0.5g mixed acid-treated carbon nanofibers into 50mL ethylene glycol, ultrasonically disperse for 5 minutes, then raise the temperature to 120°C, add 0.9mL 0.2M Na 2 CO 3 The aqueous solution was filtered after constant temperature for 1 hour, washed with water, and dried to obtain the catalyst precursor. The obtained precursor was placed in a tubular heating furnace, and the temperature was raised to 400°C at 3°C / min in a high-purity nitrogen atmosphere, kept for 4 hours, and then switched to nitrogen and hydrogen mixed gas for reduction for 1 hour to obtain carbon nanofiber-supported metal nickel catalyst. ICP results showed that the mass percent content of metallic nickel was 6.0%. The XRD calculation results show that the average particle size of metallic nickel particles is 5.1...

Embodiment 3

[0028] (1) The carbon nanofiber activation treatment is the same as in Example 1.

[0029] (2) Preparation of carbon nanofiber-supported metal nickel catalyst

[0030] Weigh 0.212g Ni(AC) 2 Add 0.5g mixed acid-treated carbon nanofibers into 50mL ethylene glycol, ultrasonically disperse for 5 minutes, then raise the temperature to 160°C, add 0.9mL 0.2M Na 2 CO 3 The aqueous solution was kept at this temperature for 1 hour, then filtered, washed with water, and dried to obtain a catalyst precursor. The obtained precursor was placed in a tubular heating furnace, and the temperature was raised to 400°C at 3°C / min in a high-purity nitrogen atmosphere, kept for 4 hours, and then switched to nitrogen and hydrogen mixed gas for reduction for 1 hour to obtain carbon nanofiber-supported metal nickel catalyst. ICP results showed that the mass percent content of metallic nickel was 6.6%. The XRD calculation results show that the average particle size of metallic nickel particles is 5...

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Abstract

The present invention is preparation process of nanometer carbon material supported metal catalyst for hydrogenating chloronitrobenzene to synthesize chloroaniline. The preparation process includes depositing nanometer carbon material, carbon nanotube or nanometer carbon fiber as carrier in water or polyol solvent to obtain catalyst precursor, and baking in high temperature inertial atmosphere to reduce in reductive atmosphere. The nanometer carbon material supported metal catalyst with metal grains dispersed homogeneously on the surface of nanometer carbon material has high catalytic activity of hydrogenating chloronitrobenzene, simple preparation process, controllable performance and other advantages. The catalyst may be also used for hydrogenating nitro compounds.

Description

technical field [0001] The invention belongs to the technical field of a catalyst for synthesizing chloroaniline by hydrogenation of chloronitrobenzene, and relates to a preparation method of a carbon nanomaterial-loaded metal catalyst for synthesizing chloroaniline by hydrogenation of chloronitrobenzene. Background technique [0002] Chloroaniline is an important class of organic chemical intermediates, widely used in the synthesis of fine chemical products such as medicine, dyes, and pesticides. At present, the synthesis of chloroaniline is mainly obtained by catalytic hydrogenation of the corresponding chloronitrobenzene. The catalysts adopted are mainly oxides, polymers and activated carbon supported noble metal catalysts such as Pt, Ru and their alloys (Appl.Catal.A 1997,164:197-203; J.Mol.Catal.A 2003,193(1- 2): 103-108; J Catal.2004,222:493-498; J Mol.Catal.A2001,170:203-208; J Col.Inter.Sci.1999 214:231-237), Raney nickel (dye Industry, 1997, 34(5): 31-33) and amor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/74B01J21/18C07C209/36C07C211/52
Inventor 邱介山王闯梁长海
Owner DALIAN UNIV OF TECH
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