Method for preparing low-temperature nitrogen-doped graphene supported nano Pd hydrogenation catalyst

A technology of nitrogen-doped graphene and hydrogenation catalyst, which is applied in hydrogenation hydrocarbon production, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of uneven particle dispersion, particle loss, and complicated operation, and achieve operational Simple, Gentle, Inexpensive Effects

Inactive Publication Date: 2014-09-10
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a kind of Method for synthesis of nitrogen-doped graphene highly dispersed Pd nanoparticle hydrogenation catalyst with relatively simple and low-cost reaction at low temperature

Method used

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  • Method for preparing low-temperature nitrogen-doped graphene supported nano Pd hydrogenation catalyst

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Experimental program
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Effect test

Embodiment 1

[0020] Weigh graphite oxide and add it to deionized water to make the concentration 2mg / mL, and ultrasonically treat it for 1.5h to obtain a highly dispersed aqueous solution of graphene oxide; add 1.85mmol ethylenediamine to the above solution, stir at room temperature for 10min, and then put it into the hydrothermal reaction In the still, crystallize at 180°C for 12h, suction filter after the crystallization, rinse the sample with deionized water, and dry at 80°C overnight to obtain nitrogen-doped graphene.

[0021] Weigh nitrogen-doped graphene and add it to deionized water (to make the concentration 1mg / mL), sonicate at 50°C for 3h, add 0.4mL PdCl 2 Aqueous solution (0.02mol / L), 1mL hydrazine hydrate was slowly added dropwise while magnetic stirring, stirred at room temperature for 30min, centrifuged, washed 5 times with water, dried in vacuum at 60°C for 2h to obtain the catalyst A.

Embodiment 2

[0023] Weigh graphite oxide and add it to deionized water (to make the concentration 2mg / mL), and ultrasonically treat it for 1.5h to obtain a highly dispersed graphene oxide aqueous solution; add 3.7mmol ammonia water to the above solution, stir at room temperature for 10min, and then put it into the hydrothermal reaction In the still, crystallize at 180°C for 12h, suction filter after the crystallization, rinse the sample with deionized water, and dry at 80°C overnight to obtain nitrogen-doped graphene.

[0024] Weigh nitrogen-doped graphene and add it to deionized water (to make the concentration 1mg / mL), sonicate at 50°C for 3h, add 0.4mL PdCl 2 Aqueous solution (0.02mol / L), 1mL of hydrazine hydrate was slowly added dropwise while stirring magnetically, stirred at room temperature for 30min, centrifuged, washed with water 5 times, and vacuum-dried at 60°C for 2h to obtain the catalyst B.

Embodiment 3

[0026] Weigh graphite oxide and add it to deionized water (to make the concentration 2mg / mL), and ultrasonically treat it for 1.5h to obtain a highly dispersed aqueous solution of graphene oxide; add 1.85mmol urea to the above solution, stir at room temperature for 10min, and then put it into the hydrothermal reaction In the kettle, it was crystallized at 180°C for 12 hours. After the crystallization was completed, it was suction-filtered, rinsed with deionized water, and dried at 80°C overnight to obtain graphene doped with different nitrogen.

[0027] Weigh nitrogen-doped graphene and add it to deionized water (to make the concentration 1mg / mL), sonicate at 50°C for 3h, add 0.4mL PdCl 2 Aqueous solution (0.02mol / L), 1mL hydrazine hydrate was slowly added dropwise while magnetic stirring, stirred at room temperature for 30min, centrifuged, washed with water 5 times, vacuum dried at 60°C for 2h to obtain the catalyst C.

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Abstract

The invention relates to a method for preparing a low-temperature nitrogen-doped graphene supported nano Pd hydrogenation catalyst. The method comprises the following steps: ultrasonically stripping graphite oxide, thereby obtaining an aqueous solution of highly dispersed graphite oxide; selecting different nitrogen sources, and synthesizing nitrogen-doped graphene at low temperature through a hydrothermal method; and performing ultrasonic treatment on the nitrogen-doped graphene, adding a certain amount of PdCl2 solution, and adding a reducing agent, thereby preparing the highly dispersed supported nano Pd hydrogenation catalyst by a chemical reduction method. Because nitrogen atoms, which contain lots of lone pair electrons and can achieve a coordination effect with metal nanoparticles, are mixed into a carbon skeleton of graphene, runoff and conglomeration of the metal nanoparticles are effectively avoided, and the dispersity of the metal nanoparticles on the surface of graphene is improved. The catalyst is used for a hydrogenation reaction of olefins and has extremely high catalytic activity and high reusability. The catalyst is simple in preparation method and low in cost, the nitrogen content is high, doped nitrogen is controllable, and industrial production is easily realized.

Description

technical field [0001] The invention relates to the technical field of hydrogenation catalysts and their preparation, in particular to a preparation method of a low-temperature nitrogen-doped graphene-loaded nano-Pd hydrogenation catalyst. Background technique [0002] Supported metals are widely used in industrially important hydrogenation reactions due to their high stability and reusability. At present, the most researched carrier for loading nanometer metals is SiO 2 、Al 2 o 3 , activated carbon, molecular sieve, etc. [0003] Graphene, also known as "single layer graphite", is SP 2 The hybridized carbon atoms are mixed into orbital domains, forming a single-layer two-dimensional crystal arranged in a honeycomb lattice structure. Its unique and perfect structure makes graphene have a large specific surface area, high electrical conductivity and good thermal stability. These properties of graphene make it an excellent carrier for nanometals. [0004] At present, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C5/03C07C9/15
Inventor 刘平武梦瑶李永昕薛冰
Owner CHANGZHOU UNIV
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