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Method for loading nano-particles of metal or metallic oxide in mesoporous silica channel

A technology of mesoporous silica and nanoparticles, applied in the field of chemical modification, can solve the problems of poor product dispersibility, waste of precursors, uneven loading, etc., and achieve the effect of mild reaction conditions and uniform loading

Active Publication Date: 2015-11-25
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the advantages of simplicity, less pollution, and low cost, and it can also overcome the defects of poor product dispersion, uneven loading, and waste of precursors prepared by existing methods.

Method used

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  • Method for loading nano-particles of metal or metallic oxide in mesoporous silica channel
  • Method for loading nano-particles of metal or metallic oxide in mesoporous silica channel
  • Method for loading nano-particles of metal or metallic oxide in mesoporous silica channel

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1, preparation spherical mesoporous silica

[0031] Weigh 0.070g of cetyltrimethylammonium bromide and disperse it in 30ml of water, stir it magnetically at a constant temperature of 60°C until it becomes a clear, transparent and uniformly dispersed solution, and then add 1ml of it with a mass fraction of 28% to the solution concentrated ammonia water (adjust the pH value of the system to 11), add 1mL of tetraethoxysilane after 10min, react for 2h, then centrifuge, wash, and dry to obtain ellipsoidal mesoporous silica with a particle size of about 100nm. The rate is 98%. Then, it was calcined at 550° C. in air for 4 hours to remove the template surfactant hexadecyltrimethylammonium bromide in the pores.

[0032] The spherical mesoporous silica transmission electron micrograph that this embodiment 1 prepares is as follows figure 1 shown. Depend on figure 1 It can be seen that the particle size of the silica ball is uniform, and the pore size is uniform.

Embodiment 2

[0033] Example 2. Preparation of mesoporous silica-based composite material loaded with metal palladium nanoparticles in the channels of mesoporous silica

[0034] Add 0.07g of surfactant cetyltrimethylammonium bromide to 30ml of deionized water, stir at a constant temperature of 60°C until the solution becomes clear and transparent, then add 1ml of concentrated ammonia water with a mass fraction of 28% ( Adjust the pH of the system to 11), add 1mL of tetraethoxysilane (TEOS) after 10min, react at 60°C for 2h under constant temperature stirring, and then add the palladium source (the palladium source is specifically ammonium chloropalladate, Add 0.18mL (0.5mol / L) into the reaction system, continue the reaction at 60°C for 20h, then centrifuge, wash, and dry to obtain an ellipsoid with palladium nanoparticles loaded in the pores with a particle diameter of about 100nm. The mesoporous silica is then calcined in a hydrogen atmosphere at 700° C. for 2 hours to remove the template ...

Embodiment 3

[0036] Example 3. Preparation of mesoporous silica-based composite material loaded with metal platinum nanoparticles in the channels of mesoporous silica

[0037]Add 0.070g of surfactant cetyltrimethylammonium bromide to 30ml of deionized water, stir at a constant temperature of 60°C until the solution becomes clear and transparent, then add 1ml of concentrated ammonia water with a mass fraction of 28% (Adjust the pH value of the system to 11), add tetraethoxysiloxane (TEOS) after 10 min to make the concentration within 1 mL, react at 60 ° C for 20 h under constant temperature stirring, and then add the platinum source (the described The platinum source is specifically chloroplatinic acid, the addition amount is 0.2mL (0.5M) into the reaction system, and the reaction is continued at 60°C for 4h, and then centrifuged, washed, and dried to obtain particles with a particle size of about 100nm. The ellipsoidal mesoporous silica of platinum nanoparticles is then calcined in a hydro...

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Abstract

The invention discloses a method for loading nano-particles of metal or metallic oxide in a mesoporous silica channel. The method comprises the following steps: taking a cation-type quaternary ammonium surfactant as a template, dispersing in water, heating and stirring until a clear and transparent solution is formed; adding an alkaline solution in the solution to adjust pH value being 9-12, adding silicon source for a first step to obtain a mesoporous silica-containing reaction system; then adding an aqueous solution of a precursor of the metal or metallic oxide to be loaded in the mesoporous silica-containing reaction system for a second step reaction to obtain the precursor silicon dioxide with the channel having uniformly loaded metal or metallic oxide, and finally roasting to obtain the mesoporous silica matrix composite material. The method has the advantages of simple operation and mild reaction condition, and supported substance distribution, loading capacity and combination can be adjusted at random according to requirement.

Description

technical field [0001] The invention belongs to the field of chemical modification, and in particular relates to a method for loading metal or metal oxide nanoparticles in the channels of mesoporous silica. Background technique [0002] As one of the most abundant substances on the earth, silica has specific properties, such as biocompatibility, stability, corrosion resistance, etc. Therefore, it can be widely used in metallurgy, machinery, chemical industry, electronics and other fields. However, since the silica naturally existing on the earth does not have a regular shape and structure, it cannot be adjusted arbitrarily during application, and cannot meet the needs of application development, so the research on synthetic silica has begun. [0003] Ordered mesoporous silica, as the name implies, refers to mesoporous silica with regular structure or regular assembly. Usually the preparation step is to use the surfactant as a template, in an acidic or alkaline environment, ...

Claims

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Application Information

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IPC IPC(8): C01B33/12B01J23/42B01J23/44B01J23/50B01J23/52B01J23/10B82Y30/00B82Y40/00
Inventor 曹安民钟爱芝万立骏
Owner INST OF CHEM CHINESE ACAD OF SCI
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