Method for preparing three-dimensional graphene supported nano Pd catalyst with soft template method and application of catalyst to nitrobenzene hydrogenation

A soft template method, graphene technology, applied in catalyst activation/preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of Pd metal particle size is too large, recycling rate Low, lamellar stacking and other problems, to achieve the effect of good catalytic activity and reusability

Active Publication Date: 2018-07-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a relatively simple, clean and low-cost preparation method for two-dimensional graphene-loaded Pd nanoparticles, which are easy to cause sheet stacking, low recycling rate, and large Pd metal particle size. Method of Pd nanoparticles / three-dimensional graphene hydrogenation catalyst for hydrogenation reaction of nitrobenzene

Method used

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  • Method for preparing three-dimensional graphene supported nano Pd catalyst with soft template method and application of catalyst to nitrobenzene hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 0.04g of graphite oxide and add it into 25mL emulsion (15mL deionized water, 5mL ethanol, 5mL cyclohexane), treat it with ultrasonic, ultrasonic frequency is 180W, room temperature ultrasonic 1.5h, then add 80mg of ascorbic acid to the solution, water bath Heat at 90°C for 0.5h, then add 0.5mL of 0.02mol / L PdCl 2 The solution was stirred and reacted in an oil bath at 100° C. for 2 hours. After the reaction, it was centrifuged, washed 5 times with deionized water and 2 times with ethanol, and dried in vacuum at 50° C. for 2 hours to obtain the catalyst A.

Embodiment 2

[0018] Weigh 0.04g of graphite oxide and add it into 16.6mL of emulsion (10mL of deionized water, 3.3mL of ethanol, 3.3mL of cyclohexane), sonicate it at an ultrasonic frequency of 180W, ultrasonicate at room temperature for 1.5h, and then add 80mg of Ascorbic acid, heated in a water bath at 90°C for 0.5h, then added 0.5mL of 0.02mol / L PdCl 2 The solution was stirred in an oil bath at 100° C. for 2 h, centrifuged after the reaction, washed 5 times with deionized water and 2 times with ethanol, and vacuum-dried at 50° C. for 2 h to obtain the catalyst B.

Embodiment 3

[0020] Weigh 0.04g of graphite oxide and add it into 8mL emulsion (6mL deionized water, 2mL ethanol, 2mL cyclohexane), treat it with ultrasonic, ultrasonic frequency is 180W, room temperature ultrasonic 1.5h, then add 80mg of ascorbic acid to the solution, water bath Heat at 90°C for 0.5h, then add 0.5mL of 0.02mol / L PdCl 2 The solution was stirred in an oil bath at 100° C. for 2 hours. After the reaction, it was centrifuged, washed 5 times with deionized water and 2 times with ethanol, and dried in vacuum at 50° C. for 2 hours to obtain the catalyst C.

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Abstract

The invention relates to a method for preparing a three-dimensional graphene supported nano Pd catalyst with a soft template method and an application of the catalyst to nitrobenzene hydrogenation. According to the method, graphene oxide is taken as a carrier precursor and dispersed in an emulsion system of water, ethanol and cyclohexane, and graphene oxide is assembled into a three-dimensional structure with ascorbic acid as a reducing agent; the high-dispersion nano Pd catalyst is prepared from three-dimensional graphene as a carrier. The catalyst is applied to the nitrobenzene hydrogenationreaction, shows high catalytic activity and stability and has higher recovery rate. The preparation conditions of the catalyst are mild, the process is simple, the cost is low, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of noble metal hydrogenation catalysts and preparation thereof, in particular to a method for preparing a three-dimensional graphene-loaded nano-Pd catalyst using a soft template and its application in hydrogenation of nitrobenzene. Background technique [0002] At present, the catalysts that can efficiently selectively catalyze the hydrogenation reaction include noble metal and non-noble metal catalysts. Noble metals have the characteristics of low loading, mild reaction conditions, and high catalytic activity. dispersion. The combination of commonly used carrier and metal is physical adsorption or agglomeration, so it is very meaningful to find a carrier that can firmly support metal nanoparticles and achieve high dispersion. [0003] As an emerging member of the carbon material family, graphene has a unique two-dimensional (2D) honeycomb lattice structure, which has excellent electronic properties and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/16B01J37/34C07C209/36C07C211/46
CPCB01J23/44B01J35/006B01J35/0066B01J37/16B01J37/343C07C209/36C07C211/46
Inventor 刘平陈炎亮张志翔李永昕
Owner CHANGZHOU UNIV
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