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Mesoporous titania material with highly crystalline framework, preparation method and application thereof

A mesoporous titanium dioxide, highly crystalline technology, applied in the field of physical chemistry, can solve the problems of pore wall collapse, affecting material structure and catalytic performance, specific surface area and pore volume decline, etc. The effect of sintering properties

Inactive Publication Date: 2015-09-23
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it can be used as a class of excellent catalytic oxidation, hydrogenation catalysts and efficient catalyst supports. However, the biggest problem in the preparation of crystalline mesoporous metal oxides is that the low hydrothermal treatment temperature (100°C) causes no The fixed pore wall structure can greatly promote the crystallization of the pore wall structure during the process of removing the template agent through high-temperature calcination, but this process often causes a large amount of collapse of the pore wall, and the specific surface area and pore volume decrease. The occurrence of this phenomenon directly affects to the structure and catalytic properties of the material

Method used

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  • Mesoporous titania material with highly crystalline framework, preparation method and application thereof
  • Mesoporous titania material with highly crystalline framework, preparation method and application thereof
  • Mesoporous titania material with highly crystalline framework, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Using polyethylene glycol-6000 as a template, DMSO as a solvent, and 180°C to synthesize CM-TiO 2 .

[0020] Add 1.0g of polyethylene glycol-6000 into 35g of dimethyl sulfoxide solvent and slightly heat to dissolve, then add 3.5g of n-butyl titanate, and at the same time add 1ml of water to promote the hydrolysis of the titanium source. After stirring and reacting at room temperature for 6 hours, the The reaction mixture was transferred into a stainless steel reaction kettle, and subjected to hydrothermal treatment at 180°C for 24 hours, then the reaction kettle was taken out, cooled, filtered with suction, washed and dried to obtain the primary product, which had a high degree of crystallinity. The primary product is calcined under air conditions at 500°C to obtain a mesoporous titanium dioxide material with open channels and highly crystallized framework. , the specific surface area of ​​the material reaches 60m 2 / g, pore diameter 18 nanometers, pore vol...

Embodiment 2

[0021] Example 2: Using polyethylene glycol-600 as a template, DMSO as a solvent, and 140°C to synthesize CM-TiO 2 .

[0022] Add 2.0g of polyethylene glycol-6000 into 90g of dimethyl sulfoxide solvent and slightly heat to dissolve, then add 3.0g of n-butyl titanate, and at the same time add about 1ml of water to promote the hydrolysis of the titanium source, stir and react at room temperature for 6 hours, Transfer the reaction mixture into a stainless steel reaction kettle, conduct hydrothermal treatment at 140°C for 24 hours, take out the reaction kettle, cool, filter with suction, wash, and dry to obtain the primary product, which has a high degree of crystallinity. The primary product is calcined under air conditions at 600°C to obtain a mesoporous titanium dioxide material with open pores and highly crystallized framework. The specific surface area of ​​the material reaches 120m 2 / g, pore diameter 4 nanometers, pore volume 0.23cm 3 / g.

Embodiment 3

[0023] Example 3: Using polyethylene glycol-2000 as a template, DMSO as a solvent, and 220°C to synthesize CM-TiO 2 .

[0024] Add 2.0g of polyethylene glycol-6000 into 90g of dimethyl sulfoxide solvent and slightly heat to dissolve, then add 3.0g of n-butyl titanate, and at the same time add about 1ml of water to promote the hydrolysis of the titanium source, stir and react at room temperature for 6 hours, Transfer the reaction mixture into a stainless steel reaction kettle, conduct hydrothermal treatment at 220°C for 24 hours, take out the reaction kettle, cool, filter with suction, wash, and dry to obtain the primary product, which has a high degree of crystallinity. The primary product is calcined under air conditions at 1000°C to obtain a mesoporous titanium dioxide material with open pores and a highly crystallized framework. The specific surface area of ​​the material reaches 50m 2 / g, pore diameter 20 nanometers, pore volume 0.1cm 3 / g.

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Abstract

The invention provides a mesoporous titania material with a high-crystallization framework and a preparation method and application thereof. The preparation method comprises the following steps: preparing a template agent solution by using industrial polyethylene glycol 800-6000 as a template agent and dimethyl sulfoxide or dimethylformamide as a solvent; adding metered titanium tetrabutoxide; self-assembling an organic template agent and inorganic substances under the high effect of a hydrogen bond between the template agent and a titanium source so as to form a basic mesoporous structure; further thermally processing through a high-temperature solvent under the temperature of 140 to 220 DEG C to crystallize the wall of mesoporous; and roasting the obtained crystallized titania primary product at high temperature of 450 to 1,000 DEG C to obtain the mesoporous titania material with opened pore canals and highly crystallized wall. The material shows high degree of crystallinity, is of a typical anatase crystal structure, has large specific surface area and adjustable pore diameter distribution, and shows relatively high catalyzing performance while catalyzing and degrading organic dye in water under an ultraviolet light condition.

Description

technical field [0001] The invention belongs to the technical fields of physical chemistry and material science, and in particular relates to a mesoporous titanium dioxide material with a highly crystalline skeleton, a preparation method and an application thereof. Background technique [0002] In recent years, mesoporous materials have been widely used in the fields of catalysts and catalyst supports, adsorption, separation, and drug sustained release, and have attracted more and more attention from scientists. Mesoporous materials have large specific surface areas and uniform And adjustable pore size and rich skeleton composition and other characteristics. However, the regular mesoporous materials with silica framework are the most reported so far, and the framework structure often exhibits an amorphous framework structure, which makes the material poor in hydrothermal stability and greatly limits its wide industrial application. [0003] In order to expand the framework ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047C02F1/30B01J21/06B01J35/10
Inventor 孔维萍刘福建王聪徐丹丹
Owner SHAOXING UNIVERSITY
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