Preparation method of palladium-mesoporous silica core-shell nano-catalytic material

A mesoporous silica, core-shell nanotechnology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problems of tedious and time-consuming preparation process

Active Publication Date: 2016-01-20
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are few related reports on palladium-mesoporous silica core-shell nanomaterials. The common synthesis method is a two-step method, that is, palladium nanoparticle solution is prepared in advance by reduction method, and then the mesoporous silica shell is coated. The preparation process is cumbersome and time-consuming

Method used

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  • Preparation method of palladium-mesoporous silica core-shell nano-catalytic material
  • Preparation method of palladium-mesoporous silica core-shell nano-catalytic material
  • Preparation method of palladium-mesoporous silica core-shell nano-catalytic material

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Embodiment 1

[0021] (1) Weigh 0.1g of CTAB, add 50mL of deionized water and 0.5mL of 1M sodium hydroxide solution to fully dissolve the template agent CTAB in an alkaline aqueous system to obtain a uniform clear liquid;

[0022] (2) After stirring at 60°C for 30 minutes, add 1.25mL of 0.1M aqueous formaldehyde solution and 1.25mL of 0.05M sodium citrate aqueous solution, and then add 1.25mL of 0.1M sodium chloropalladate Na 2 PdCl 4 aqueous solution, so that formaldehyde and sodium citrate reduce sodium chloropalladate to palladium nanoparticles;

[0023] (3) After stirring for 15 minutes at 60°C, add a mixture of 0.5g tetraethyl orthosilicate and 1.5g ethanol, and continue stirring at 80°C for 2 hours to crosslink the tetraethyl orthosilicate and the surfactant CTAB micelles , the palladium core is coated with a mesoporous silica shell. The resulting precipitate was centrifuged, washed three times with water, then washed twice with ethanol, dried in an oven at 50°C overnight, and baked ...

Embodiment 2

[0025] (1) Weigh 0.075g of CTAB, add 50mL of deionized water and 0.4mL of 1M sodium hydroxide solution to fully dissolve the template agent CTAB in an alkaline aqueous system to obtain a uniform clear liquid;

[0026] (2) After stirring at 60°C for 30 minutes, add 0.375mL of 0.1M formaldehyde aqueous solution and 1.5mL of 0.05M sodium citrate aqueous solution, and then add 0.75mL of 0.1M palladium chloride PdCl 2 Aqueous solution, make formaldehyde and sodium citrate reduce palladium chloride into palladium nanoparticles;

[0027] (3) After stirring for 15 minutes at 60°C, add a mixture of 0.6g tetraethyl orthosilicate and 1.5g ethanol, and continue stirring at 80°C for 2 hours to crosslink the tetraethyl orthosilicate and the surfactant CTAB micelles , the palladium core is coated with a mesoporous silica shell. The resulting precipitate was centrifuged, washed three times with water, then washed twice with ethanol, dried overnight at 50°C in an oven, and baked in a muffle f...

Embodiment 3

[0029] (1) Weigh 0.125g of CTAB, add 50mL of deionized water and 0.6mL of 1M sodium hydroxide solution to fully dissolve the template agent CTAB in an alkaline aqueous system to obtain a uniform clear liquid;

[0030] (2) After stirring at 60°C for 30 minutes, add 0.75mL of 0.1M aqueous formaldehyde solution and 1.5mL of 0.05M sodium citrate aqueous solution, and then add 1.0mL of 0.1M sodium chloropalladate Na 2 PdCl 4 aqueous solution, so that formaldehyde and sodium citrate reduce sodium chloropalladate to palladium nanoparticles;

[0031] (3) After stirring for 15 minutes at 60°C, add a mixture of 0.4g tetraethyl orthosilicate and 1.5g ethanol, and continue stirring at 80°C for 2 hours to crosslink the tetraethyl orthosilicate and the surfactant CTAB micelles , the palladium core is coated with a mesoporous silica shell. The resulting precipitate was centrifuged, washed three times with water, then washed twice with ethanol, dried overnight at 50°C in an oven, and baked ...

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Abstract

The invention discloses a preparation method of a palladium-mesoporous silica core-shell nano-catalytic material. Sodium hydroxide is taken as a catalyst, CTAB (cetyltrimethylammonium bromide) is taken as a template of a mesostructure, formaldehyde and sodium citrate are taken as reducing agents, and a palladium-mesoporous silica nano-material with a core-shell structure is obtained through a simple and convenient synthetic route in one step. The preparation method comprises the following steps: firstly, CTAB as the template is dissolved sufficiently in an alkaline aqueous system; then formaldehyde and sodium citrate are added and reduce a palladium source into palladium nano-particles; finally, tetraethoxysilane is cross-linked with CTAB micelle as a surfactant, a palladium core is coated with a mesoporous silica shell layer, and the palladium-mesoporous silica core-shell nano-material can be obtained. The precious metal palladium has very good catalytic activity, so that mesoporous channels of the silica shell layer can provide channels allowing molecules to enter, leave or be contacted with the active core, and the palladium-mesoporous silica core-shell material can be applied to the field of catalysis.

Description

technical field [0001] The invention belongs to the technical field of nano-core-shell materials, and in particular relates to a preparation method of a palladium-mesoporous silicon oxide core-shell nano-catalysis material. Background technique [0002] Nanocomposites with a core-shell structure not only have the functions of the core and the shell, but also prevent the agglomeration or deformation of the nanocore, and are widely used in catalysis, biomedicine, energy storage, and adsorption. The metal nanoparticles are coated with a porous shell layer, which can provide channels for molecules to enter and exit and contact the active core while separating the active nanoparticle core. Among them, the noble metal palladium has good catalytic activity, and the mesoporous silica material has ordered mesoporous channels, high specific surface area, uniform pore size, large pore volume, controllable shape, high thermal stability and easy surface modification. Porous shell materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44
Inventor 何丹农陈俊琛李玉真张春明
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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