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Nitrogen-doped ordered mesoporous carbon-loaded nano-palladium material and preparation method thereof

A mesoporous carbon and nitrogen doping technology, applied in the field of materials, can solve the problems of catalyst metal palladium loss, easy poisoning and deactivation, agglomeration, etc., and achieves the effects of simple equipment requirements, low price and simple operation.

Inactive Publication Date: 2019-08-23
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, silica or other inert substances are usually used as the carrier, and the binding force between the carrier and the precious metal palladium is weak. During the reaction, the catalyst has problems such as metal palladium loss, agglomeration, and easy poisoning and deactivation.

Method used

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  • Nitrogen-doped ordered mesoporous carbon-loaded nano-palladium material and preparation method thereof
  • Nitrogen-doped ordered mesoporous carbon-loaded nano-palladium material and preparation method thereof
  • Nitrogen-doped ordered mesoporous carbon-loaded nano-palladium material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] A preparation of nitrogen-doped ordered mesoporous carbon-supported nano-palladium material, the specific steps are as follows:

[0039] (1) At 45°C, put 12.0mmol of phenol into a volumetric flask and stir until dissolved; add 30mL of sodium hydroxide solution, and after 10min to 15min, add 4.0mL of formaldehyde solution to adjust the temperature at 65°C to 70°C to obtain For pink solution A (resole phenolic resin), dissolve 1.93g of F127 in 30mL of water to obtain solution B, add solution B to A, add 100mL of water, stir for 14-16 hours and then red precipitate appears, stop the reaction;

[0040] (2) Then add 85mL of the reaction solution obtained above into the hydrothermal kettle, add 280mL of water, and heat at 130°C for 24h;

[0041] (3) Suction filter the hydroheated solution and then dry it in vacuum at 80°C, add 0.8g of urea and 0.5g of the obtained dried material and calcinate to 400°C to obtain a black powder, and then use 0.05g / mL palladium chloride ethanol ...

Embodiment 2

[0044] A preparation of nitrogen-doped ordered mesoporous carbon-supported nano-palladium material, the specific steps are as follows:

[0045] (1) At 45°C, put 12.0mmol of phenol into a volumetric flask and stir until dissolved; add 30mL of sodium hydroxide solution, and after 10min to 15min, add 4.0mL of formaldehyde solution to adjust the temperature at 65°C to 70°C to obtain For pink solution A (resole phenolic resin), dissolve 1.93g of F127 in 30mL of water to obtain solution B, add solution B to A, add 100mL of water, stir for 14-16 hours and then red precipitate appears, stop the reaction;

[0046] (2) Then add 85mL of the reaction solution obtained above into the hydrothermal kettle, add 280mL of water, and heat at 130°C for 24h;

[0047] (3) Suction filter the hydroheated solution and then dry it in vacuum at 80°C, add 0.8g of urea and 0.4g of the dried material and calcinate to 400°C to obtain a black powder, then use 0.1g / mL palladium chloride ethanol solution Afte...

Embodiment 3

[0050] A preparation of nitrogen-doped ordered mesoporous carbon-supported nano-palladium material, the specific steps are as follows:

[0051] (1) At 45°C, put 12.0mmol of phenol into a volumetric flask and stir until dissolved; add 30mL of sodium hydroxide solution, and after 10min to 15min, add 4.0mL of formaldehyde solution to adjust the temperature at 65°C to 70°C to obtain For pink solution A (resole phenolic resin), dissolve 1.93g of F127 in 30mL of water to obtain solution B, add solution B to A, add 100mL of water, stir for 14-16 hours and then red precipitate appears, stop the reaction;

[0052] (2) Then add 85mL of the reaction solution obtained above into the hydrothermal kettle, add 280mL of water, and heat at 130°C for 24h;

[0053] (3) Suction filter the hydroheated solution and then dry it in vacuum at 80°C, add 0.8g of urea and 0.4g of the dried material and calcinate to 400°C to obtain a black powder, then use 0.3g / mL palladium chloride ethanol solution Afte...

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Abstract

The invention belongs to the technical field of the mesoporous material preparation, and relates to a nitrogen-doped ordered mesoporous carbon-loaded nano-palladium material and a preparation method thereof. The material has a three-dimensional cubic mesostructure, a large specific surface area (100-200 m2 / g), a large pore volume (0.1-1.0 cm<3> / g), and a uniform pore diameter (2-3 nm), the nitrogen content is controlled to be 9 wt%, the size of the palladium nanoparticles is uniform and controllable (0.1-2 nm), and the palladium content is controlled to be 0.2-5 wt%. The preparation method comprises the following steps: mixing and stirring a pre-synthesized low-grade phenolic resin and a F127 aqueous solution at a certain temperature for 14-16 h, then performing low concentration hydrothermal treatment for 24 h, performing vacuum drying for 12 h, performing calcination on the material together with a nitrogen-containing small molecule under the nitrogen protection to obtain a brown powder, performing immersion in a palladium chloride ethanol solution, and performing the mixed reduction of hydrogen and nitrogen to obtain the ordered mesoporous carbon material-loaded palladium catalyst. The prepared material can be used in the selective hydrogenation reaction of phenol, cinnamaldehyde and the like. The preparation method of the catalytic material is simple, the cost is low, and the equipment requirements are simple and convenient.

Description

technical field [0001] The invention belongs to the field of materials, and relates to an ordered mesoporous carbon material, in particular to a nitrogen-doped ordered mesoporous carbon supported nano palladium material and a preparation method thereof. Background technique [0002] The preparation of supported metal catalysts usually has the problem of uneven metal size distribution or large metal particles. This inhomogeneity affects the efficient utilization of metal active sites and thus reduces the selectivity to specific products in reactions. This is because only a small fraction of metal particles with suitable size distribution in the catalyst can serve as catalytically active sites, and other larger-sized particles may be inert or cause undesired side reactions during the reaction. Recent theoretical and experimental studies have shown that subnanometer-sized metal clusters and catalysts with well-defined single-site catalysts have better catalytic activity or sel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10B01J37/02B01J37/03B01J37/10C07C5/08C07C5/09
CPCB01J27/24B01J37/10B01J37/031B01J37/0018B01J37/0201C07C5/08C07C5/09B01J35/39B01J35/615B01J35/633B01J35/635B01J35/647
Inventor 万颖李顺林朱晓雨
Owner SHANGHAI NORMAL UNIVERSITY
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