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Nitrogen-doped carbon-loaded palladium catalyst as well as preparation method and application thereof

A nitrogen-doped carbon and palladium catalyst technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as complex process, poor recyclability, and poor catalyst stability

Active Publication Date: 2022-02-18
TAIZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned method is complex, and the stability of Pd in ​​the prepared catalyst is relatively poor, and then its recyclability is poor, and the activity of the catalyst is not high enough.

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  • Nitrogen-doped carbon-loaded palladium catalyst as well as preparation method and application thereof
  • Nitrogen-doped carbon-loaded palladium catalyst as well as preparation method and application thereof

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preparation example Construction

[0024] The invention provides a method for preparing a nitrogen-doped carbon-supported palladium catalyst, comprising the following steps:

[0025] Mix the carbon material with a strong acid solution and perform acid treatment to obtain an acid-activated carbon material;

[0026] The acid-activated carbon material, the water-soluble palladium salt solution and the nitrogen-containing ionic liquid are mixed and then dried to obtain a catalyst precursor;

[0027] The catalyst precursor is calcined and then reduced under a protective atmosphere to obtain a nitrogen-doped carbon-supported palladium catalyst.

[0028] The invention mixes the carbon material with a strong acid solution and performs acid treatment to obtain the acid-activated carbon material.

[0029] In the present invention, the carbon material preferably includes activated carbon, mesoporous carbon, carbon nanotube or graphene, more preferably activated carbon. In the present invention, the strong acid solution ...

Embodiment 1

[0055] (1) Put 1 g of activated carbon in 30 mL of nitric acid-hydrochloric acid mixed solution, carry out acid treatment under stirring conditions for 10 h and then filter, wash and dry the obtained solid components to obtain acid-activated activated carbon, wherein the nitric acid in the mixed solution of nitric acid-hydrochloric acid And the concentration of hydrochloric acid is 2mol / L;

[0056] (2) Dissolve 1g of palladium chloride in 2mL of concentrated hydrochloric acid, transfer to a 100mL volumetric flask, add deionization to constant volume, and obtain a chloropalladium acid solution with a concentration of 10mg / mL;

[0057] (3) 1 g of the acid-activated activated carbon, 1.71 mL of the chloropalladium acid solution and 300 mg of 1,3-diethylimidazole acetate were mixed and stirred at room temperature for 1 h, and then dried at 130° C. for 10 h while stirring, Obtain catalyst precursor;

[0058] (4) The catalyst precursor is heated to 800°C at a rate of 5°C / min in a n...

Embodiment 2

[0061] (1) Put 1 g of activated carbon in 30 mL of nitric acid-hydrochloric acid mixed solution, carry out acid treatment under stirring conditions for 10 h and then filter, wash and dry the obtained solid components to obtain acid-activated activated carbon, wherein the nitric acid in the mixed solution of nitric acid-hydrochloric acid And the concentration of hydrochloric acid is 2mol / L;

[0062] (2) Dissolve 1g of palladium chloride in 2mL of concentrated hydrochloric acid, transfer to a 100mL volumetric flask, add deionization to constant volume, and obtain a chloropalladium acid solution with a concentration of 10mg / mL;

[0063] (3) 1 g of the acid-activated activated carbon, 1.71 mL of the chloropalladium acid solution and 400 mg of 1,3-diethylimidazole acetate were mixed and stirred at room temperature for 1 h, and then dried at 130° C. for 10 h while stirring, Obtain catalyst precursor;

[0064] (4) The catalyst precursor is heated to 800°C at a rate of 5°C / min in a n...

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Abstract

The invention provides a nitrogen-doped carbon-loaded palladium catalyst as well as a preparation method and application thereof, and belongs to the technical field of catalysts. The preparation method of the nitrogen-doped carbon-loaded palladium catalyst comprises the following steps: mixing a carbon material and a strong acid solution, and carrying out acid treatment to obtain an acid-activated carbon material; mixing the acid activated carbon material, a water-soluble palladium salt solution and a nitrogen-containing ionic liquid, and drying the material to obtain a catalyst precursor; and calcining the catalyst precursor in a protective atmosphere, and reducing to obtain the nitrogen-doped carbon-loaded palladium catalyst. In the method, the acid treatment can increase the number of oxygen-containing functional groups on the surface of the carbon material and improve the dispersion stability of palladium nanoparticles; secondly, the nitrogen-containing ionic liquid is used as a precursor of nitrogen, nitrogen atoms generated by decomposition in the calcining process are doped, so that nitrogen can be uniformly doped in the carbon material, meanwhile, the dispersity and the stability of palladium nanoparticles are improved, and the catalytic activity is high. The preparation method is simple in process and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a nitrogen-doped carbon-supported palladium catalyst and a preparation method and application thereof. Background technique [0002] Cyclohexanecarboxylic acid is an important chemical and pharmaceutical intermediate. In chemical industry, it can be used as clarifier of petroleum, pesticide, solubilizer of heat-cured rubber and dye additive, etc. It can also be used to synthesize photocuring agent l-hydroxycyclohexyl phenyl ketone; in pharmaceutical intermediates, cyclohexyl Formic acid can be used to synthesize drugs such as praziquantel, caprolactam and acesulfame potassium, and the economical and efficient synthesis of cyclohexanecarboxylic acid has high significance and value. [0003] The most direct and effective method for the synthesis of cyclohexanecarboxylic acid and benzoic acid is the selective hydrogenation of benzene ring under the action of a catalyst. At prese...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J23/44B01J37/06B01J37/08B01J37/18C07C67/303C07C69/75
CPCB01J27/24B01J23/44B01J37/06B01J37/086B01J37/18C07C67/303C07C2601/14C07C69/75
Inventor 韩得满李嵘嵘陈先朗武承林
Owner TAIZHOU UNIV
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