Nitrogen-doped carbon material-supported palladium-based catalyst as well as preparation method and application thereof

A technology of carbon materials and nitrogen doping, applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problems of expensive raw materials, complicated preparation, lack of research on doped nitrogen species, etc., to achieve Simple operation, easy operation, practical effect

Inactive Publication Date: 2017-11-03
SHAANXI SCI TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both the in-situ doping method and the post-treatment method have the problems of expensive raw materials and complicated preparation
[0005] Based on the reported template method to prepare nitrogen-doped carbon materials, all of them focus on the construction of material pore structure (Vinu, A.; Ariga, K.; Mori, T.; Nakanishi, T.; Hishita, S.; Golberg, D.;Bando, Y. Preparation and Characterization of Well-Ordered Hexagonal Mesoporous Carbon Nitride. Adv. Mater. 2005, 17, 1648-1652), but there is a lack of research on doped nitrogen species, especially the preparation of nitrogen-doped carbon materials There is even a blank in the application of supported catalysts in the hydrogenation of formic acid from carbon dioxide

Method used

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  • Nitrogen-doped carbon material-supported palladium-based catalyst as well as preparation method and application thereof
  • Nitrogen-doped carbon material-supported palladium-based catalyst as well as preparation method and application thereof
  • Nitrogen-doped carbon material-supported palladium-based catalyst as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Add 3.35g of diethylenetriamine (a) and 5.0g of carbon tetrachloride into a round bottom flask containing 0.5g of SBA15, heat up to 90ºC and reflux for 4h to obtain a brown solid, put it in an oven for 100ºC to dry for 12h, put Put it into a tube furnace and heat up to 400ºC at 2.5ºC / min in a nitrogen atmosphere to polymerize for 4 hours. After cooling to room temperature, remove the template with 8 wt % hydrofluoric acid, wash and dry, and obtain a black nitrogen-doped carbon material NC-a -400.

[0044] Analyze the relevant performance parameters of the nitrogen-doped carbon material NC-a-400, such as Figure 1~7 shown. The specific surface area of ​​the nitrogen-doped carbon material NC-a-400 is 296m 2 / g, the pore volume is 0.35cm 3 / g, the pore size is 4.6nm; SEM figure shows that from the XPS peak fitting figure of N1s, it can be seen that there are mainly two types of N, which are pyridine nitrogen at 398.3 eV and pyrrole nitrogen at 400.4 eV nitrogen.

[00...

Embodiment 2

[0048] Add 4.77g of triethylenetetramine (b) and 5.0g of carbon tetrachloride into a round bottom flask containing 0.5g of SBA15, raise the temperature to 100ºC and reflux for 4h to obtain a dark brown solid, put it in an oven and dry it at 100ºC for 12h. Put it into a tube furnace and heat up to 500ºC at 3.0ºC / min in a nitrogen atmosphere to polymerize for 4 hours. After cooling to room temperature, remove the template with 8 wt % hydrofluoric acid, wash and dry, and obtain a black nitrogen-doped carbon material NC- b-500.

[0049] In a 250 ml round bottom flask, add 0.5 g of the new nitrogen-doped carbon material NC-b-500, 100 ml of absolute ethanol, ultrasonically shake for 20 min, add PdCl containing 20 mg of palladium 2 solution, ultrasonically oscillated for 20 min, heated to reflux and stirred for 12 h, added 15 ml 1 M / L NaBH 4 , continue to stir for 1h, cool, filter, wash, and vacuum-dry to obtain the palladium catalyst Pd / NC-b-500 supported by the novel nitrogen-dope...

Embodiment 3

[0052] Add 6.2g of tetraethylenepentamine (c) and 5.0g of carbon tetrachloride into a round-bottomed flask containing 0.5g of SBA15, heat up to 110ºC and reflux for 5h to obtain a dark brown solid, which is dried in an oven at 100ºC for 12h. Put it into a tube furnace and heat up to 600ºC at 4.0ºC / min in a nitrogen atmosphere to polymerize for 5 hours. After cooling to room temperature, remove the template with 8 wt % ammonium fluoride, wash and dry, and obtain a new black nitrogen-doped carbon material NC -c-600.

[0053] In a 250 ml round bottom flask, add 0.5 g of the new nitrogen-doped carbon material NC-c-600, 100 ml of propanol, ultrasonically shake for 20 min, add PdCl containing 30 mg of palladium 2 solution, ultrasonically oscillated for 20 min, heated to reflux and stirred for 12 h, added 20ml 1 M / L NaBH 4 , continue to stir for 1 h, cool, filter, wash, and vacuum-dry to obtain palladium catalyst Pd / NC-c-600 supported by a novel nitrogen-doped carbon material. The ...

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Abstract

The invention discloses a nitrogen-doped carbon material-supported palladium-based catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps: adding a nitrogen-doped carbon material into an alcohol solution; performing ultrasonic treatment for 5 min to 30 min; adding 1 wt% to 4.2 wt% of a palladium precursor solution to obtain an unreduced catalyst; heating, refluxing and stirring the unreduced catalyst for 4 h to 12 h; adding 10 ml to 20 ml of 1 M / L NaBH4; continuing to stir for 1 h to 2 h; filtering, washing and drying in vacuum to obtain the nitrogen-doped carbon material-supported palladium-based catalyst. In the invention, the catalyst nitrogen uses a nitrogen-doped carbon material as a catalyst carrier; the noble metal palladium is dispersed on the carrier; the loading capacity of palladium in the catalyst is 1.0 wt% to 5.0 wt%. The catalyst provided by the invention is applied to an aspect of catalyzing preparation of formate, and has advantages of simple production, low price of used materials, strong catalytic activity, high reusability and simple operation.

Description

technical field [0001] The invention belongs to the field of compound reaction catalysts, and in particular relates to a palladium-based catalyst supported on a nitrogen-doped carbon material and its preparation method and application. Background technique [0002] Porous carbon materials have a series of characteristics such as developed pores, high specific surface area, good chemical stability, acid and alkali resistance, high temperature resistance, electrical conductivity, heat conduction and low cost, and are one of the indispensable and important materials in modern industry. It is used in the fields of electrode materials (such as fuel cells, supercapacitors, etc.), adsorption materials, energy storage materials, and catalyst carriers. [0003] In recent years, nitrogen-doped carbon materials have developed rapidly, mainly because the introduction of nitrogen atoms into the carbon skeleton has a great influence on the properties of carbon materials. Nitrogen atoms w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C51/41C07C53/06
CPCB01J27/24C07C51/41C07C51/412C07C53/06
Inventor 邵先钊季晓晖王伟田光辉刘军海郑楠
Owner SHAANXI SCI TECH UNIV
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