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Preparation of nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst and application thereof in catalyzing o-chloronitrobenzene hydrogenation reaction

A nano-catalyst, core-shell structure technology, applied in the preparation of organic compounds, the preparation of amino compounds, catalysts for physical/chemical processes, etc., can solve the problems of poor stability, easy agglomeration and deactivation, expensive precious metal catalysts, etc., and achieve high stability. properties, high catalytic activity, enhanced electron transport properties, and effects of chemical reactivity

Active Publication Date: 2017-05-31
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to provide a self-reduction method for preparing a non-noble metal alloy nanocatalyst with a core-shell structure, which solves the problems of expensive metal catalysts, easy agglomeration and deactivation, poor stability, and the need for additional reducing agents. Catalytic hydrogenation of nitro compounds to generate haloanilines

Method used

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  • Preparation of nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst and application thereof in catalyzing o-chloronitrobenzene hydrogenation reaction
  • Preparation of nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst and application thereof in catalyzing o-chloronitrobenzene hydrogenation reaction
  • Preparation of nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst and application thereof in catalyzing o-chloronitrobenzene hydrogenation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 4.04gFe(NO 3 ) 3 9H 2 O, 8.724gNi(NO 3 ) 2 ·6H 2 O was dissolved in 100mL deionized water, ultrasonicated for 5min, mixed thoroughly, and recorded as solution A.

[0026] 2.56 g NaOH and 125 μL of 30% H 2 o 2Dissolved in 100mL deionized water, ultrasonicated for 5min, mixed thoroughly, and recorded as solution B.

[0027] Slowly mix the two solutions at room temperature and add them to the colloid mill at a controlled speed of 3000rpm. After stirring vigorously for 2 minutes, transfer them to a polytetrafluoroethylene liner. After airtight, statically crystallize at room temperature for 24 hours. After the reaction, centrifuge and wash To neutrality, freeze-dry to obtain the NiFe-LDH precursor of the nanocatalyst.

[0028] Take 0.5g of NiFe-LDH, 0.19g of dicyandiamide and 1.31g of melamine and grind them thoroughly in a mortar until they are evenly mixed. -1 Heating up to 500°C and keeping it warm for 6 hours, after grinding, a nano-catalyst with a core-shell s...

Embodiment 2

[0032] 4.04gFe(NO 3 ) 3 9H 2 O, 5.816gNi(NO 3 ) 2 ·6H 2 O was dissolved in 100mL deionized water, ultrasonicated for 5min, mixed thoroughly, and recorded as solution A.

[0033] 2.56 g NaOH and 125 μL of 30% H 2 o 2 Dissolve in 100mL deionized water, sonicate for 5min, and mix well. Denoted as solution B.

[0034] The two solutions were slowly mixed at room temperature and added to the colloid mill at a controlled speed of 3000 rpm. After being vigorously stirred for 2 minutes, they were transferred to a polytetrafluoroethylene liner. After airtight, they were statically crystallized at room temperature for 24 hours. After the reaction is finished, it is centrifuged and washed to neutrality, and freeze-dried to obtain the -LDH precursor of the nanocatalyst.

[0035] Take 0.5g of NiFe-LDH, 0.19g of dicyandiamide and 1.31g of melamine and grind them thoroughly in a mortar until they are evenly mixed. -1 Raise the temperature to 500°C and keep it warm for 6h, and get th...

Embodiment 3

[0038] 4.04gFe(NO 3 ) 3 9H 2 O, 11.632gNi(NO 3 ) 2 ·6H 2 O was dissolved in 100mL deionized water, ultrasonicated for 5min, mixed thoroughly, and recorded as solution A.

[0039] 2.56 g NaOH and 125 μL of 30% H 2 o 2 Dissolved in 100mL deionized water, ultrasonicated for 5min, mixed thoroughly, and recorded as solution B.

[0040] The two solutions were slowly mixed at room temperature and added to the colloid mill at a controlled speed of 3000rpm. After being vigorously stirred for 2 minutes, they were transferred to a polytetrafluoroethylene liner. After airtight, they were statically crystallized at room temperature for 24 hours. After the reaction is finished, it is centrifuged and washed to neutrality, and freeze-dried to obtain the LDH precursor of the nanocatalyst.

[0041] Take 0.5g NiFe-LDH, 0.19g dicyandiamide and 1.31g melamine and grind them thoroughly in a mortar until they are evenly mixed, place them in a porcelain boat, raise the temperature to 500°C at...

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Abstract

The invention provides a preparation method of a nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst and the application of the nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst in catalyzing an o-chloronitrobenzene hydrogenation reaction. According to the method, the novel nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst is prepared by synthesizing a ferronickel layered doubled hydroxide precursor with small grain size and high surface energy through a nucleation crystallization isolation method, evenly mixing the ferronickel layered doubled hydroxide precursor with a melamine and dicyandiamide mixed carbon material precursor, and finally self-reducing at high temperature. The nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst is efficiently applied to the reaction where halogenated aniline is generated through catalytic hydrogenation of a nitro-halogen compound, and the conversion rate of o-chloronitrobenzene and the selectivity of o-chloroaniline are respectively up to 95-100% and 98-100%. The structure of the novel nitrogen doped carbon-encapsulated core-shell structure ferro-nickel nano-catalyst is unique and novel, the process is green and energy-saving, the structure of the catalyst is stable, and the catalyst has a broad application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to the preparation of a nitrogen-doped carbon-coated core-shell structure nickel-iron alloy nano-catalyst and a method for the hydrogenation reaction of o-chloronitrobenzene. Background technique [0002] Aromatic halogenated anilines have important applications in pharmaceutical synthesis, dyes, medicines, etc., but in the process of generating halogenated anilines by catalytic hydrogenation of halogenated nitro compounds, the breakage of C-Cl bonds is relatively easy to occur, resulting in halogenated The yield of aniline is greatly reduced. Therefore, the selective hydrogenation of halonitro compounds to generate haloanilines is particularly important. People often use noble metal catalysts such as Pd, Au, Pt, etc. for this reaction (J.Lyu, J.Wang, C.Lu, L.Ma, Q.Zhang, X.He, and X.Li.Size-dependent halogenated nitrogen Hydrogenation selectivity of Pdnanoparticles[...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10B82Y30/00B82Y40/00C07C209/36C07C211/52
CPCB82Y30/00B82Y40/00C07C209/36B01J27/24B01J35/615C07C211/52
Inventor 李峰刘春玲范国利杨兰
Owner BEIJING UNIV OF CHEM TECH
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