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Ordered alumina mesoporous material and preparation method thereof

A technology of mesoporous materials and sequenced alumina, which is applied in the field of mesoporous materials, can solve the problems of lowering, collapse of ordered mesoporous structures, specific surface area and pore volume, achieve high catalytic activity, and the preparation method is simple and easy repeat effect

Active Publication Date: 2017-08-04
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the application of EISA method to prepare ordered alumina mesoporous materials requires strict control of the temperature and relative humidity during the solvent volatilization process, and the pore walls of the obtained materials are still mainly composed of amorphous hydroxyl aluminum, which is very easy to occur during high-temperature calcination. Crystalline phase transition, resulting in partial collapse of the ordered mesoporous structure and significant reduction in specific surface area and pore volume

Method used

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  • Ordered alumina mesoporous material and preparation method thereof
  • Ordered alumina mesoporous material and preparation method thereof
  • Ordered alumina mesoporous material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Under vigorous stirring at 30°C, add 3.5g of EO to 20mL of absolute ethanol solution containing 0.6g of citric acid and 2.0g of 12M hydrochloric acid 106 PO 70 EO 106 and 4.08g of aluminum isopropoxide were completely dissolved to obtain a clear solution; the resulting clear solution was poured into a sealed autoclave for solvothermal pretreatment at 100°C for 24 hours; subsequently, the obtained sol was volatilized in an open state at 60°C Treatment for 24 hours; finally, the obtained solid sample was calcined at 550°C for 5 hours to remove the organic template existing in the mesoporous channels to obtain an alumina mesoporous material sample with a highly ordered two-dimensional hexagonal mesoporous structure.

[0029] figure 1 The XRD spectrum of the sample prepared above is given. It can be seen from the figure that the obtained material shows a strong diffraction peak and a relatively weak diffraction peak at 0.90° and 1.56°, respectively. By calculating the r...

Embodiment 2

[0035] Under vigorous stirring at 40°C, add 4.0 g of EO to 20 mL of absolute ethanol solution containing 0.8 g of oxalic acid and 2.6 g of 2M nitric acid 106 PO 70 EO 106 and 7.1g of aluminum nitrate were completely dissolved to obtain a clear solution; the resulting clear solution was poured into a sealed autoclave and subjected to solvothermal pretreatment at 60°C for 24 hours; subsequently, the obtained sol was subjected to solvent volatilization treatment at 45°C for 48 hours ; Finally, the obtained solid sample was calcined at 550° C. for 5 h to remove the organic template existing in the mesoporous channels, and obtain the ordered alumina mesoporous material sample.

[0036] The results of XRD and nitrogen adsorption characterization show that the prepared sample has a highly regular and ordered two-dimensional hexagonal mesoporous channel structure. The specific surface area and pore volume of the sample are calculated to be 302 m 2 / g and 0.52cm 3 / g, the mesopore d...

Embodiment 3

[0041] Under strong stirring at 35°C, add 3.6g EO to 20mL absolute ethanol solution containing 1.0g glacial acetic acid and 3.0g 6M hydrochloric acid 20 PO 70 EO 20 and 4.5g of aluminum tert-butoxide, completely dissolved to obtain a clear solution; the resulting clear solution was poured into a sealed autoclave, and subjected to solvothermal pretreatment at 100°C for 24 hours; subsequently, the obtained sol was volatilized in an open state at 80°C Treat for 24 hours; finally, the obtained solid sample is calcined at 600° C. for 5 hours to remove the organic template existing in the mesoporous channel, and obtain the ordered alumina mesoporous material sample.

[0042] The results of XRD and nitrogen adsorption characterization show that the prepared sample has a highly regular and ordered two-dimensional hexagonal mesoporous channel structure. According to calculation, the specific surface area and pore volume of the sample are 350m 2 / g and 0.73cm 3 / g, the mesopore diame...

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Abstract

The invention relates to an ordered alumina mesoporous material and a preparation method thereof. The preparation method comprises the following steps: dissolving an inorganic acid, an organic carboxylic acid, a block copolymer non-ionic surfactant and an aluminum source in anhydrous alcohol, heating and pretreating in a sealed high-pressure environment, evaporating out the solvent in an open state, and calcining at 400-650 DEG C to obtain the ordered alumina mesoporous material. The mesoporous material prepared in the invention has a highly ordered two-dimensional hexagonal mesoporous structure, large specific surface area and pore volume, and high thermal stability; the specific surface area is adjustable in a range of 200-450 m<2> / g, the pore volume is adjustable in a range of 0.3-1.2 cm<3> / g, and the mesoporous size is adjustable in a range of 5.0-20.0 nm; and after the mesoporous material is calcined at 1000 DEG C for 1 h, the structure and properties do not change, and the specific surface area and the pore volume are reduced to less than 40% and 47%, respectively.

Description

technical field [0001] The invention relates to a mesoporous material, in particular to a mesoporous alumina material and a preparation method thereof. The mesoporous alumina material of the present invention has highly regular and orderly mesoporous structure, adjustable pore diameter, high specific surface area and pore volume, and high thermal stability. Background technique [0002] Ordered alumina mesoporous materials are ideal catalysts or catalyst support materials due to their highly regular pore structure, large specific surface area and pore volume, concentrated pore distribution, and adjustable acidity. , adsorption and separation, host-guest assembly, and nanoreactors have broad application prospects. [0003] At present, the synthesis of ordered alumina mesoporous materials mainly adopts the "soft template method", that is, an appropriate amount of surfactant is dissolved in a specific solvent to form micelles as an organic template for guiding the mesoporous s...

Claims

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Application Information

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IPC IPC(8): C01F7/02B01J21/04B01J32/00B01J35/10
CPCC01F7/02B01J21/04C01P2006/17C01P2002/72B01J35/638B01J35/635B01J35/633B01J35/615B01J35/647
Inventor 潘大海朱淑英陈树伟于峰崔杏雨陈伟李瑞丰
Owner TAIYUAN UNIV OF TECH
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