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Preparation method for ordered mesoporous gamma-Al2O3

A technology of ordered mesoporous and mesoporous, which is applied in the field of preparation of ordered mesoporous γ-Al2O3, can solve the problems of complex process, low thermal stability, and small specific surface of mesoporous alumina, and achieve large specific surface area and pore diameter Narrow distribution effect

Inactive Publication Date: 2012-04-25
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent CN101024503A (application number 200710063718.5) uses aluminum nitrate as the aluminum source and ammonium carbonate as the precipitating agent to prepare ordered mesoporous alumina by using high-gravity technology.
Chinese patent CN101597077A (Application No. 200910069671.2) provides a technology for preparing ordered mesoporous alumina using sodium lauroyl glutamate as a surfactant. The disadvantage is that the obtained mesoporous alumina has a small specific surface area and low thermal stability.
Most of the products obtained by the above methods are amorphous mesoporous alumina, the pore structure is worm-like, the specific surface is small, and the thermal stability is low.
Therefore, the application of mesoporous alumina in high-temperature catalytic reactions and high-temperature assembly is limited.

Method used

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  • Preparation method for ordered mesoporous gamma-Al2O3
  • Preparation method for ordered mesoporous gamma-Al2O3
  • Preparation method for ordered mesoporous gamma-Al2O3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A. Synthesis reaction: Dissolve 1.0 g of P123 in 20 mL of absolute ethanol, add mixed acid (concentrated hydrochloric acid: citric acid: glacial acetic acid = 2:1:2) while stirring, and adjust the pH to 3~4. After clarification, add 10 mmol aluminum isopropoxide, seal with PE film, and continue to stir for 5 h.

[0027] B. Aging: Put the solution in step A into aging for 10 h to obtain a transparent gel.

[0028] C. Drying: transfer the gel in step B to a 60 °C oven for 48 h to obtain a white powder.

[0029] D. Calcination: heat the white powder in step C to 550°C at a rate of 1°C / min in an oxygen atmosphere for 6 hours, then raise the temperature to 700°C at a rate of 10°C / min and hold for 1 hour.

[0030] The product obtained by this method is ordered mesoporous γ-Al 2 o 3 , the small angle XRD pattern of this product ( figure 1 ) and TEM ( figure 2 ) It can be seen that the product channels are arranged in a two-dimensional regular hexagon, and the order i...

Embodiment 2

[0032] A. Synthesis reaction: Dissolve 1.0 g P123 in 20 mL of absolute ethanol, add mixed acid (concentrated nitric acid: citric acid: glacial acetic acid = 2.5:1:1) while stirring, and adjust the pH to 3~4. After clarification, add 10 mmol aluminum isopropoxide, seal with PE film, and continue to stir for 5 h.

[0033] B. Aging: Put the solution in step A into aging for 10 h to obtain a transparent gel.

[0034] C. Drying: transfer the gel in step B to a 60 °C oven for 48 h to obtain a white powder.

[0035] D. Calcination: heat the white powder in step C to 550°C at a rate of 1°C / min in an oxygen atmosphere for 6 hours, then raise the temperature to 700°C at a rate of 10°C / min and hold for 1 hour.

[0036] Mesoporous γ-Al 2 o 3 The specific surface area is 293.7 m 2 / g, pore volume 0.49 m 3 / g, and the average pore diameter is 9.9 nm. The product has better orderliness than the product of Embodiment 1, as shown by the XRD figure ( figure 2 )As can be seen.

Embodiment 3

[0038] A. Synthesis reaction: Dissolve 1.0 g P123 in 20 mL absolute ethanol, add mixed acid (concentrated hydrochloric acid: citric acid: glacial acetic acid = 2:1:2) while stirring, and adjust the pH to 3~4. After clarification, add 10 mmol aluminum isopropoxide, seal with PE film, and continue to stir for 5 h.

[0039] B. Aging: Put the solution in step A into aging for 10 h to obtain a transparent gel.

[0040] C. Drying: transfer the gel in step B to a 60 °C oven for 48 h to obtain a white powder.

[0041] D. Calcination: heat the white powder in step C to 550°C at a rate of 1°C / min in an oxygen atmosphere and keep it for 6 hours, then raise the temperature to 1000°C at a rate of 10°C / min and hold it for 1 hour.

[0042] Mesoporous γ-Al 2 o 3 The specific surface area is 181.23 m 2 / g, pore volume 0.23 m 3 / g, and the average pore diameter is 7.3 nm. The ordered mesoporous structure is still maintained, and the order is lower than that of Embodiment 1.

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Abstract

The invention discloses a preparation method for ordered mesoporous gamma-Al2O3. The preparation method comprises the steps of a synthesis reaction, aging, drying and calcining so as to obtain the ordered mesoporous gamma-Al2O3. The method provided in the invention is simple and easily practicable, is safe to operate and is easy for industrial production; the obtained gamma-Al2O3 has the advantages of a large specific surface and high thermostability.

Description

technical field [0001] The invention relates to the technical field of preparation of mesoporous materials, in particular to an ordered mesoporous γ-Al 2 o 3 method of preparation. Background technique [0002] In 1992, the scientists of Mobil Corporation used alkyl quaternary ammonium salt cationic surfactants as templates for the first time to successfully synthesize the M41S series of silicon-based mesoporous molecular sieves under alkaline conditions. The materials industry attaches great importance to it. Various non-silicon-based mesoporous materials have been developed successively, including transition metal oxides, rare earth oxides and composite metal oxides. Because mesoporous materials have larger pore diameter, specific surface area and pore volume, higher thermal stability and hydrothermal stability, the pore size can be adjusted according to different experimental conditions. Therefore, it has a wide range of applications in macromolecular catalysis, bio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/02
Inventor 刘应亮余彩霞阳区
Owner JINAN UNIVERSITY
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