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A kind of ordered alumina mesoporous material and preparation method thereof

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

Active Publication Date: 2018-10-02
山西泰亨科技有限公司
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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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  • A kind of ordered alumina mesoporous material and preparation method thereof
  • A kind of ordered alumina mesoporous material and preparation method thereof
  • A kind of ordered alumina mesoporous material and preparation method thereof

Examples

Experimental program
Comparison scheme
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. Inorganic acid, organic carboxylic acid, block copolymer nonionic surfactant and aluminum source are dissolved in absolute ethanol, and the solvent heat is sealed under high pressure. Pretreatment, evaporating the solvent in an open state, and calcining at 400 to 650°C to obtain ordered alumina mesoporous materials. The mesoporous material prepared by the invention has a highly ordered two-dimensional hexagonal mesoporous structure, large specific surface area and pore volume, and high thermal stability. Its specific surface area is 200-450m2 / g, and the pore volume is 0.3-1.2 cm3 / g, the mesopore diameter is adjustable in the range of 5.0~20.0nm. After high-temperature roasting at 1000°C for 1 hour, the structural properties did not change, and the specific surface area and pore volume decreased by 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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Patent Type & Authority Patents(China)
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 山西泰亨科技有限公司