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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has the advantages of simplicity, less pollution, and low cost, and it can also overcome the

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

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Example Embodiment

[0030] Example 1. Preparation of spherical mesoporous silica

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

[0032] The transmission electron micrograph of the spherical mesoporous silica prepared in Example 1 is as follows figure 1 Shown. by figure 1 It can be seen that the particle size of the silica balls is uniform, and the pore size is uniform.

Example Embodiment

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

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

Example Embodiment

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

[0037] Add 0.070g of surfactant cetyltrimethylammonium bromide to 30ml of deionized water, stir at a constant temperature of 60℃, until the solution becomes clear and transparent, add 1ml of 28% concentrated ammonia water to it (Adjust the pH of the system to 11), add tetraethoxysiloxane (TEOS) after 10 minutes to make the concentration within 1 mL, react at 60°C for 20 hours under constant temperature stirring, and then calculate the amount of platinum source (the said The platinum source, specifically chloroplatinic acid, was added to the reaction system in an amount of 0.2mL (0.5M), and the reaction was continued at 60°C for 4 hours, and then centrifuged, washed, and dried to obtain a pore with a particle size of about 100nm. The ellipsoidal mesoporous silica of platinum nanoparticles is then calcined at 700°C in a hydrogen atmos...

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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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