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Preparation of a nitrogen-doped carbon-coated core-shell nickel-iron alloy nanocatalyst and its application in the hydrogenation of o-chloronitrobenzene

A nano-catalyst, o-chloronitrobenzene technology, applied in the preparation of organic compounds, preparation of amino compounds, physical/chemical process catalysts, etc., can solve the problems of easy agglomeration and deactivation, expensive noble metal catalysts, poor stability, etc., to achieve High catalytic activity, enhanced electron transport properties and chemical reactivity, high stability effects

Active Publication Date: 2019-06-07
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 a nitrogen-doped carbon-coated core-shell nickel-iron alloy nanocatalyst and its application in the hydrogenation of o-chloronitrobenzene
  • Preparation of a nitrogen-doped carbon-coated core-shell nickel-iron alloy nanocatalyst and its application in the hydrogenation of o-chloronitrobenzene
  • Preparation of a nitrogen-doped carbon-coated core-shell nickel-iron alloy nanocatalyst and its application in the hydrogenation of o-chloronitrobenzene

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-coated core-shell structure nickel-iron alloy nanocatalyst in the field of catalyst technology and its application in catalyzing the hydrogenation reaction of o-chloronitrobenzene. The method first synthesizes a nickel-iron layered double metal hydroxide precursor with small particle size and high surface energy through a nucleation and crystallization isolation method, and then uniformly mixes it with a melamine and dicyandiamide mixed carbon material precursor. , and finally a new type of nitrogen-doped carbon-coated core-shell structure nickel-iron alloy nanocatalyst was prepared through high-temperature self-reduction. It is efficiently used in the catalytic hydrogenation of halogenated nitro compounds to produce halogenated anilines. The conversion rate of o-chloronitrobenzene and the selectivity of o-chloroaniline can reach 95-100% and 98-100% respectively. . This new nitrogen-doped carbon-coated core-shell structure nickel-iron alloy nanocatalyst has a novel and unique structure, a green and energy-saving process, and a stable catalyst structure, and has broad application prospects.

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 Patents(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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