Preparation method of macroporous-mesoporous alumina

A mesoporous alumina and aluminum salt technology, applied in the direction of alumina/aluminum hydroxide, can solve the problem of inability to realize the controllable adjustment of macropore-mesoporous aperture, and achieve the effect of reducing preparation cost and simple process

Inactive Publication Date: 2010-10-20
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the size of the macropore (300nm or 400nm) is completely determined by the size of the polystyrene droplet introduced twice, that is, the size of the macropore depends on the size of the polystyrene droplet
The pore size cannot be adjusted by partially changing the components of the solution itself and the interaction of organic molecules in the system
Huining Li et al. (Inorganic Chemistry, 2009, 48:4421) also used the sol-gel method to introduce polymethyl methacrylate (PMMA) droplets with a single dispersed phase into the mixed solution using F127 as a template to achieve large Pore-the formation of macropores in mesoporous alumina, the disadvantage is that the size of the macropores is completely determined by the size of the secondary introduction of polymethyl methacrylate droplets, which cannot be achieved by partially changing the components of the solution system itself The adjustment of the pore size is used to realize the formation of the macropore-mesopore composite pore structure, so it is impossible to realize the controllable adjustment of the macropore-mesopore diameter. In the process of use, especially for the macromolecular catalytic process of complex components limitations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 1.7g citric acid and 7.5g Al(NO 3 ) 3 9H 2 O was dissolved in 40 mL of anhydrous ethanol solution, stirred at a constant speed at room temperature for 0.5 h, the solution was colorless and transparent, then 2.0 g of P123 was added to the above solution, and stirred for 24 h in a water bath at 60 °C. Move the above mixed solution to a 60°C oven to continue aging treatment, and gradually remove ethanol and water in the system to obtain a macroporous-mesoporous alumina precursor, a macroporous-mesoporous alumina precursor that completely removes ethanol and water It is light yellow and transparent, ground into white powder, and placed in a program-controlled muffle furnace for high temperature treatment at a heating rate of 1°C / min, 400°C for 4 hours, and then naturally cooled to obtain a macroporous-mesoporous alumina material.

[0019] A transmission microscope shows that the obtained macroporous-mesoporous alumina material has a macropore diameter of 60-80 nm an...

Embodiment 2

[0021] Weigh 1.3g lauric acid and 5.0g AlCl 3 ·6H 2 O was dissolved in 40 mL of absolute ethanol solution, stirred at a constant speed at room temperature for 0.5 h, the solution was colorless and transparent, then 1.6 g of P123 was added to the above solution, and stirred for 24 h in a water bath at 30 °C. Move the above mixed solution to a 60°C oven to continue aging treatment, and gradually remove ethanol and water in the system to obtain a macroporous-mesoporous alumina precursor, a macroporous-mesoporous alumina precursor that completely removes ethanol and water It is light yellow and transparent, ground into white powder, and placed in a program-controlled muffle furnace for high-temperature treatment at a heating rate of 1°C / min, and then kept at 400°C for 4 hours to obtain a macroporous-mesoporous alumina material.

[0022] A transmission microscope shows that the obtained macroporous-mesoporous alumina material has a macropore diameter of 50-80 nm and a mesopore dia...

Embodiment 3

[0024] Weigh 1.5g citric acid and 7.5g Al(NO 3 ) 3 9H 2 O was dissolved in 40mL of absolute ethanol solution, stirred at a constant speed at room temperature for 0.5h, the solution was colorless and transparent, then 2.4g of F127 was added to the above solution, and stirred in a water bath at 50°C for 24h. Move the above mixed solution to a 60°C oven to continue aging treatment, and gradually remove ethanol and water in the system to obtain a macroporous-mesoporous alumina precursor, a macroporous-mesoporous alumina precursor that completely removes ethanol and water It is light yellow and transparent, ground into white powder, and placed in a program-controlled muffle furnace for high-temperature treatment at a heating rate of 1°C / min, and then kept at 400°C for 4 hours to obtain a macroporous-mesoporous alumina material.

[0025] A transmission microscope shows that the obtained macroporous-mesoporous alumina material has a macropore diameter of 50-80 nm and a mesopore dia...

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Abstract

The invention provides a preparation method of macroporous-mesoporous alumina, which comprises the following steps: a, dissolving reaction assistants and aluminum salts into solution of an organic solvent, wherein the molar ratio of the reaction assistants and aluminum ions is (3-5): 1, dissolving a template agent into the solution, wherein the molar ratio of the aluminum ions and the template agent is 1: (0.015-0.025), and finally controlling the PH value of the solution to be 3.5-6.0; b, aging the solution prepared in Step a to gradually remove the organic solvent and water in the system, thereby obtaining a macroporous-mesoporous alumina precursor; c, calcinating at the temperature of 400-800 DEG C, thereby obtaining macroporous-mesoporous alumina powder. The invention has the advantages of simple process, regular pore canals and centralized pore size distribution, and can realize controlled regulation according to specific application conditions. Therefore, the invention has significant value of application in heterogeneous catalysis and adsorptive separation in the petrochemical industry and the use as the catalyst carrier, energy material and the like.

Description

technical field [0001] The invention relates to a preparation method of macroporous-mesoporous alumina. Background technique [0002] Activated alumina can be widely used as catalytic materials, such as acid catalysts, catalyst supports, and in the fields of adsorption and separation. Compared with traditional alumina, alumina porous materials are expected to replace traditional activated alumina due to their outstanding characteristics such as large specific surface area, regular structure, large pore size, and acid centers on the surface, and can be used in heterogeneous catalysis and adsorption separation in the petrochemical field. And as a catalyst carrier and energy material. [0003] At present, scholars at home and abroad are in the exploratory stage for the synthesis of porous alumina, mainly focusing on the preparation and regulation of the morphology of single mesoporous alumina with ordered channels and regular pore diameters. Compared with alumina materials wi...

Claims

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Application Information

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IPC IPC(8): C01F7/02
Inventor 杨华明刘明珠欧阳静
Owner CENT SOUTH UNIV
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