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

A particle size, oxide technology, used in chemical instruments and methods, iron oxides, carbon compounds, etc., can solve problems such as limited effectiveness, and achieve the effect of improving application performance, simple operation, and easy implementation.

Active Publication Date: 2012-12-05
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

Examples

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Effect test

preparation example Construction

[0021] Below according to existing preparation method, in conjunction with our invention, the present invention is described in further detail:

[0022] A method for preparing an ordered mesoporous metal oxide material with adjustable particle size, comprising 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 dissolves, then add ethyl orthosilicate and stir at 25-35°C for 12-24 hours , and then transfer the mixture to a hydrothermal reaction kettle for 1-4 days at 100-130°C, then filter, wash, dry and calcinate at 350-600°C for 2-5 hours in an air atmosphere to remove the surfactant after natural cooling Obtain a white powder sample for subsequent 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 tetraethyl orthosilicate, P123, hydro...

Embodiment 1

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

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

[0033] Use 3g of the above-mentioned ordered mesoporous silica as a hard template, disperse it into 60g of ethanol, add 9g of ferric nitrate, stir and impregnate at room temperature, so that the iron precursor is immersed in the mesoporous pores...

Embodiment 2

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

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

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

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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 that adjusts the particle size of the ordered mesoporous metal oxide material prepared by adjusting the state of the calcination container. Background technique [0002] Ordered mesoporous metal oxide materials have attracted extensive attention due to their applications in the fields of optics, electricity, magnetism, catalysis, and sensing. The most direct method to synthesize 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 the nanocasting method (Nanocasting), also known as the hard template method, which is a method that can prepare ordered mesoporous metal oxide materials with a wider composition range, mainly based on ...

Claims

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Application Information

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Patent Type & Authority Applications(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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