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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AI-Extracted 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-th...

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.

Application Domain

Aluminium oxides/hydroxides

Technology Topic

PetrochemicalAluminum Ion +5

Examples

Experimental program(4)

Example Embodiment

[0017] Example 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 for 0.5 h at room temperature, 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 the aging treatment, and gradually remove the ethanol and water in the system to obtain a macroporous-mesoporous alumina precursor, which completely removes ethanol and water. The macroporous-mesoporous alumina precursor It is light yellow and transparent, ground into a white powder, and then placed in a program-controlled muffle furnace for high temperature treatment. The heating rate is 1 °C/min, and the temperature is kept at 400 °C for 4 hours, and then naturally cooled to obtain macroporous-mesoporous alumina materials.

[0019] Transmission microscope shows that the macroporous-mesoporous alumina material has a macropore diameter of 60-80 nm and a mesopore diameter of 20-40 nm. N 2 The gas adsorption and desorption analysis results show that its specific surface area is 290m 2 /g, the mesopores are concentrated at 30 nm, and the macropores are concentrated at 70 nm.

Example Embodiment

[0020] Example 2

[0021] Weigh 1.3g lauric acid and 5.0g AlCl 3 ·6H 2 O was dissolved in 40 mL of anhydrous ethanol solution, stirred at a constant speed for 0.5 h at room temperature, 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 the aging treatment, and gradually remove the ethanol and water in the system to obtain a macroporous-mesoporous alumina precursor, which completely removes ethanol and water. The macroporous-mesoporous alumina precursor It is light yellow and transparent, ground into a white powder, and then placed in a program-controlled muffle furnace for high temperature treatment.

[0022] Transmission microscope shows that the macroporous-mesoporous alumina material has a macropore diameter of 50-80 nm and a mesopore diameter of 3-5 nm. N2 gas adsorption and desorption analysis results show that its specific surface area is 320m 2 /g, the mesopores are concentrated at 3.7nm, and the macropores are concentrated at 55nm.

Example Embodiment

[0023] Example 3

[0024] Weigh 1.5g 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 for 0.5 h at room temperature, the solution was colorless and transparent, then 2.4 g of F127 was added to the above solution, and stirred for 24 h in a water bath at 50 °C. Move the above mixed solution to a 60°C oven to continue the aging treatment, and gradually remove the ethanol and water in the system to obtain a macroporous-mesoporous alumina precursor, which completely removes ethanol and water. The macroporous-mesoporous alumina precursor It is light yellow and transparent, ground into a white powder, and then placed in a program-controlled muffle furnace for high temperature treatment.

[0025] Transmission microscope shows that the macroporous-mesoporous alumina material has a macropore diameter of 50-80 nm and a mesopore diameter of 10-30 nm. N 2 The results of gas adsorption and desorption analysis show that its specific surface area is 260m 2 /g, the mesopores are concentrated at 15 nm, and the macropores are concentrated at 80 nm.

PUM

Property	Measurement	Unit
Large hole diameter	60.0 ~ 80.0	nm
Mesopore diameter	20.0 ~ 40.0	nm
Specific surface area	290.0	m²/g

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Simple process
low cost of preparation

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

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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