Supported non-noble metal catalyst and preparation and application thereof

A non-precious metal and catalyst technology, applied in the field of supported non-precious metal catalyst and its preparation and application, can solve the problems of expensive graphene carrier, low product yield, stoichiometric and unfriendly environment, etc., and achieve excellent recycling performance , the effect of high catalytic activity

Active Publication Date: 2016-07-13
DALIAN 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

There are many problems in the traditional synthesis method (coupling reaction between amine compounds and diazonium salts): 1. The product yield is low; 2. The oxidants that are stoichiometric and environmental

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Weigh 130.5 mg of cobalt acetate, 221.6 mg of o-phenanthroline, and 50 mL of absolute ethanol into a round bottom flask, and stir for a period of time. Then 0.94 g of magnesium hydroxide was weighed and added to the above solution, ultrasonicated for a period of time, and then stirred and refluxed at 60° C. for 4 hours. Use a rotary evaporator to remove ethanol from the refluxed catalyst solution at 40-50° C. to obtain a solid, which is dried in an oven at 80° C. overnight. Then the catalyst was ground, put into a quartz boat, and calcined at 800° C. for 2 hours under inert components to obtain a Co-N-C / MgO catalyst with a loading capacity of 3 wt%, which was marked as 1# catalyst.

[0029] Electron microscope analysis shows that the particle size of the Co nanoparticles is about 4.0 nm, and the particle size is small and uniformly dispersed.

Embodiment 2

[0030] Example 2: Weigh 128.7 mg of cobalt acetate, 333.4 mg of o-phenanthroline, and 50 mL of absolute ethanol into a round bottom flask, and stir for a period of time. Then 4 g of magnesium hydroxide was weighed and added to the above solution, ultrasonicated for a period of time, and then stirred and refluxed at 60° C. for 4 hours. Use a rotary evaporator to remove ethanol from the refluxed catalyst solution at 40-50° C. to obtain a solid, which is dried in an oven at 80° C. overnight. Then the catalyst was ground, put into a quartz boat, and calcined at 700°C for 2 hours under inert components to obtain a Co-N-C / MgO catalyst with a loading capacity of 0.68 wt%, which was marked as 2# catalyst.

[0031] Electron microscope analysis shows that the particle size of the Co nanoparticles is smaller than 2.0 nm, and the particle size is small and uniformly dispersed.

Embodiment 3

[0032] Example 3: Weigh 126 mg of cobalt acetate, 450.7 mg of o-phenanthroline, and 50 mL of absolute ethanol into a round bottom flask, and stir for a period of time. 1 g of magnesium aluminum hydrotalcite was weighed and added to the above solution, ultrasonicated for a period of time, and then stirred and refluxed at 60° C. for 4 hours. Use a rotary evaporator to remove ethanol from the refluxed catalyst solution at 40-50° C. to obtain a solid, which is dried in an oven at 80° C. overnight. Then the catalyst was ground, put into a quartz boat, and calcined at 700° C. for 2 hours under inert components to obtain a Co-N-C / HT catalyst with a loading capacity of 2 wt%, marked as 3# catalyst.

[0033] Electron microscope analysis shows that the particle size of the Co nanoparticles is about 5 nm, and the particle size is small and uniformly dispersed.

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Abstract

A supported non-noble metal catalyst used for preparation of an azo compound from an aromatic nitro compound by hydrogenation coupling is disclosed, an active component of the supported non-noble metal catalyst is any one or more than two of Co, Mn, Fe, Ni and Cu, a carrier is a nitrogen-doped carbon-inorganic oxide composite, the content of the active component in the catalyst is 0.1-15wt%, and an inorganic oxide is any one of alumina, aluminum hydroxide, magnesium oxide, magnesium hydroxide, silica, SBA-15, magnesium aluminum hydrotalcite, titanium oxide and cerium oxide. A preparation process is as follows: the active component and a nitrogen-containing complex are together impregnated on the inorganic oxide, and then calcined at certain temperature. The catalyst has excellent catalytic performance in the preparation of the azo compound from a nitro compound by selective hydrogenation coupling one-step method. The catalyst is simple in preparation, and has high catalytic activity and stability.

Description

technical field [0001] The invention relates to a supported non-precious metal catalyst, its preparation method and its application in the preparation of azo compounds by hydrogenation coupling of aromatic nitro compounds. Background technique [0002] The development of efficient and stable supported non-noble metal catalysts to replace noble metal catalysts has always been an important research direction in the field of catalysis. Compared with noble metals (such as Pt, Pd, Ru, Rh, Ir, etc.), non-noble metals (Fe, Co, Ni, Cu, etc.) are not only abundant and cheap, but also show better stability than noble metal catalysts in many reactions. and selectivity, such as Fischer-Tropsch synthesis, ORR catalyst for oxygen reduction reaction, cycloaddition reaction, C-C bond coupling reaction, etc. Therefore, it is of great significance to study the preparation methods of new non-noble metal catalysts and expand their catalytic potential for the development of green, efficient and...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J29/035C07C245/08
Inventor 王爱琴刘文刚张磊磊张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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