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Preparation method of alumina with intensive mesopore diameter distribution

A technology of pore size distribution and alumina, which is applied in the field of metal organic compound synthesis, can solve the problem that it is difficult to obtain mesoporous alumina with highly ordered pores, it is impossible to obtain mesoporous alumina materials, and it is impossible to form bulk mesoporous alumina, etc. problems, to achieve the effect of no environmental pollution and toxic residues, easy filtration, and narrow pore size distribution

Inactive Publication Date: 2011-07-13
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of mesoporous alumina by electrochemical method has the disadvantages of low yield and high energy consumption, and it cannot form bulk mesoporous alumina
When surfactants are used as templates, it is difficult to obtain mesoporous alumina with highly ordered channels, and due to the shortcomings of the surfactant "soft" template method, it is impossible to obtain mesoporous alumina with both crystalline skeleton and regular channel structure. Porous alumina material

Method used

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  • Preparation method of alumina with intensive mesopore diameter distribution
  • Preparation method of alumina with intensive mesopore diameter distribution

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Put 27g of aluminum ingots, 1.33g of anhydrous aluminum trichloride and 51g of n-butanol (water content less than 0.2%) in a 1L four-neck flask with a condenser tube, after reflux reaction for 1h, add 320g of n-butanol and 160g of boiling range It is a mixture of solvent oil at 160°C-165°C, reflux for 18h, and filter while it is hot. Put the filtrate into a 2L four-necked bottle with a temperature of 80°C, add 400g of deionized water at a temperature of 80°C, heat up to 90°C, perform a hydrolysis reaction for 4 hours, separate the alcohol and solvent oil, and then add 500g of deionized water at 95°C, Raise the temperature to 115-180°C, age for 14 hours, distill off the remaining alcohol and solvent oil, and dry at 120°C for 6 hours to obtain 60g of white alumina. After analysis by XRD, differential heat, ICP-MS and BET method, it is proved to be mesoporous alumina, and the purity of alumina is greater than 99.9%.

Embodiment 2

[0017] Put 27g of aluminum ingots, 1.33g of anhydrous aluminum trichloride and 51g of n-pentanol (water content less than 0.2%) in a 1L four-neck flask with a condenser tube, after reflux for 0.5h, add 390g of n-amyl alcohol and 220g of boiling water The process is 160°C-165°C solvent oil, reflux for 0.5h, and filter while it is hot. Put the filtrate into a 2L four-necked bottle with a temperature of 80°C, add 400g of deionized water at a temperature of 80°C, heat up to 90°C, perform a hydrolysis reaction for 4 hours, separate the alcohol and solvent oil, and then add 500g of deionized water at 95°C, Raise the temperature to 115-180°C, age for 14 hours, distill off the remaining alcohol and solvent oil, and dry at 120°C for 6 hours to obtain 60g of white alumina. After analysis by XRD, differential heat, ICP-MS and BET method, it is proved to be mesoporous alumina, and the purity of alumina is greater than 99.9%.

Embodiment 3

[0019] Put 27g of aluminum wire, 1.3g of anhydrous aluminum trichloride and 50g of n-hexanol in a 2L four-neck flask. After reacting for 0.5h, add 460g of n-hexanol and 255g of solvent oil, reflux for 2h, and filter while it is hot. Add 400g of deionized water at 90°C to a 2L four-necked bottle at 90°C, stir and hydrolyze for 2 hours, separate the alcohol, then add 500g of 95°C deionized water, age for 16 hours, distill off the remaining alcohol and solvent oil, 120°C After drying for 6 hours, 60 g of white alumina was obtained. After XRD, differential thermal and ICP-MS analysis, it is proved to be mesoporous alumina, and the purity of alumina is greater than 99.9%.

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Abstract

The invention provides a preparation method of alumina with intensive mesopore diameter distribution, belonging to the technical field of metal organic synthesis. The preparation method comprises the following steps: carrying out a reaction on metallic aluminum the purity of which is more than 99.5% and C4-C8 alcohol to prepare alkoxyaluminium; and hydrolyzing, aging and drying the alkoxyaluminium so as to obtain the mesopore alumina with the pore diameter of 3-20 nm. By using the preparation method, the defects that template agent and other auxiliaries are added in mesopore alumina preparation and then are removed through a calcination method are overcome. The aluminum with various mesopore sizes and 99.9% purity can be obtained through selecting different alcohols and hydrolysis control conditions. The preparation method has the advantages of simplified process, high preparation efficiency and low preparation cost.

Description

technical field [0001] The invention discloses a method for preparing alumina with concentrated mesopores, which belongs to the technical field of synthesis of metal organic compounds. Its preparation method is to use metal aluminum and C4-C8 alcohol as reactants, anhydrous aluminum chloride as catalyst, synthesize alkoxy aluminum, obtain aluminum hydroxide through hydrolysis of alkoxy aluminum, and obtain mesopore diameter concentration after aging and drying alumina. Alcohol and water produced after hydrolysis and aging can be recycled. This method has no environmental pollution and toxic residues. The obtained product has high purity and concentrated pore size distribution. The product is widely used in the field of catalyst carriers. Background technique [0002] Mesopore is also called mesopore, which refers to the pore size of 2 to 50nm. Mesoporous alumina has a unique pore structure, large specific surface area, high mechanical strength and other excellent characteri...

Claims

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Application Information

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IPC IPC(8): C01F7/42
Inventor 辛秀兰徐培力徐培全徐宝财
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY