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Method for preparing ordered mesoporous metal oxide material with adjustable particle size

A technology of particle size and oxide, applied in the direction of chemical instruments and methods, iron oxide, carbon compounds, etc., can solve the problems of limited effectiveness and achieve the effect of improving application performance, simple operation, and easy realization

Active Publication Date: 2014-04-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the effectiveness of these methods is limited. The particle size of the ordered mesoporous metal oxide materials prepared by the current nanocasting method is much smaller than that of the silicon oxide template, often between 50-300nm.
This limits the further improvement of the application performance and the further expansion of the application field of ordered mesoporous metal oxide materials to a certain extent.

Method used

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  • Method for preparing ordered mesoporous metal oxide material with adjustable particle size
  • Method for preparing ordered mesoporous metal oxide material with adjustable particle size
  • Method for preparing ordered mesoporous metal oxide material with adjustable particle size

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preparation example Construction

[0021] The following is a further detailed description of the present invention based on the existing preparation method and our invention:

[0022] A preparation method of ordered mesoporous metal oxide material with adjustable particle size, which comprises the following steps:

[0023] 1) Preparation of ordered mesoporous silica template material: mix and stir the surfactant, water, butanol and hydrochloric acid until the surfactant is dissolved, then add ethyl orthosilicate and stir at 25-35°C for 12-24 hours , Then transfer the mixture to a hydrothermal reactor for 1-4 days at 100-130°C. After cooling naturally, it will be filtered, washed, dried and calcined in an air atmosphere at 350-600°C for 2-5 hours to remove the surfactant. Obtain a white powder sample for use;

[0024] The surfactant is a triblock copolymer P123(OH(CH 2 CH 2 O) 20 (CH 2 CH(CH 3 )O) 70 (CH 2 CH 2 O) 20 H,MW=5800);

[0025] The molar ratio of the ethyl orthosilicate, P123, hydrochloric acid, water, and bu...

Embodiment 1

[0031] Example 1, by controlling the volume of the calcining vessel (the vessel volume is from 1.5ml to 20ml to 700ml), the prepared ordered mesoporous Fe 2 O 3 The particle size of the material.

[0032] Mix 6g of surfactant P123, 217g of water, 6g of butanol and 11.8g of hydrochloric acid (concentration of 35%) until the surfactant is dissolved, then add 12.9g of ethyl orthosilicate and stir at 35°C for 12 hours. The mixture was transferred to a hydrothermal reactor and reacted at 120°C for 1 day. After natural cooling, it was filtered, washed, dried and calcined in an air atmosphere at 400°C for 3 hours to remove the surfactant to obtain a white powder of ordered mesoporous silica for use. ;

[0033] Using 3g of the above ordered mesoporous silica as a hard template, disperse it in 60g of ethanol, add 9g of ferric nitrate, stir and impregnate at room temperature, so that the iron precursor is immersed in the silica mesoporous channels, and then the ethanol solvent is evaporated....

Embodiment 2

[0034] Example 2, by controlling the size of the opening of the calcining vessel (from completely closed, to 50% open to completely open), the prepared ordered mesoporous In 2 O 3 The particle size of the material.

[0035] Mix 6g of surfactant P123, 217g of water, 6g of butanol and 11.8g of hydrochloric acid (concentration of 35%) until the surfactant is dissolved, then add 12.9g of ethyl orthosilicate and stir at 35°C for 12 hours. The mixture was transferred to a hydrothermal reactor and reacted at 120°C for 1 day. After natural cooling, it was filtered, washed, dried and calcined in an air atmosphere at 400°C for 3 hours to remove the surfactant to obtain a white powder of ordered mesoporous silica for use. ;

[0036] Using 3g of the above ordered mesoporous silica as a hard template, disperse it in 60g of ethanol, add 9g of indium nitrate, and stir and impregnate at room temperature so that the indium precursor is immersed in the mesoporous channels of the silica, and then the...

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Abstract

The invention relates to a method for preparing an ordered mesoporous metal oxide material with adjustable particle size. According to the method, an ordered mesoporous silica material which is synthesized in advance is taken as a hard template, the growth of a crystal in the calcining process is controlled by controlling the volume of a container in a calcining step, and the volume of the calcining container is in inverse proportion to the particle size of ordered mesoporous metal oxide; the particle size of the ordered mesoporous metal oxide is smaller when the container is larger; when the volume of the calcining container is the same, the growth of the crystal in the calcining process is controlled by controlling the size of an opening of the container in the calcining step, and the size of the opening of the calcining container is in inverse proportion to the particle size of the ordered mesoporous metal oxide; and the particle size of the ordered mesoporous metal oxide is smaller when the opening is larger. The method is easy to operate and implement, additional synthesis steps are not needed, and the application performance of the prepared ordered mesoporous metal oxide material is improved.

Description

Technical field [0001] The invention belongs to the field of preparation of inorganic porous materials. More specifically, it relates to a hard template nano-casting method for the ordered mesoporous metal oxide material prepared by adjusting the state of the calcining container. Background technique [0002] Ordered mesoporous metal oxide materials have attracted widespread attention due to their applications in the fields of light, electricity, magnetism, catalysis and sensing. The most direct method for synthesizing ordered mesoporous metal oxides is the surfactant-directed self-assembly method, also known as the soft template method, which is similar to the preparation method of mesoporous silicates. Another alternative preparation method is nanocasting, also known as hard template method. It is a method that can prepare ordered mesoporous metal oxide materials with a wider range of composition, mainly with ordered mesoporous Silica such as SBA-15 and KIT-6 are used as hard...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/14C01G49/06C01G51/04C01G15/00C01B32/384
Inventor 孙晓红季惠明李晓雷
Owner TIANJIN UNIV
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