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One step method for preparing high specific surface area micro/meso porous aluminate

A high specific surface area, mesoporous aluminate technology, applied in chemical instruments and methods, molecular sieve compounds, inorganic chemistry, etc., can solve the problems of easy product agglomeration, high cost, small specific surface area, etc., and achieve mild reaction conditions and save energy. The effect of production energy consumption and simple production process

Inactive Publication Date: 2007-05-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of preparing this type of spinel material is mainly the traditional ceramic method, but because the product is easy to agglomerate when calcined at high temperature, the overall uniformity is poor, and the specific surface area is also small, it is difficult to have porous characteristics such as micropores and mesoporous, serious have greatly affected the application of this type of material
So far, there has been no report on the synthesis of mesoporous aluminates using supramolecular self-assembly of surfactants, which is mainly due to the structure and composition of spinel-type composite metal oxides compared with single metal oxides. It is more complicated, and the preparation conditions are much harsher, usually requiring high-temperature calcination above 700 ° C, which leads to the easy destruction of the mesoporous channel structure
Currently such as literature O.R. Evans, A.T.Bell and T.D.Tilley, J.Catal.226, 292 (2004) and literature M.A.Valenzulela, P.Boshch, G.Aguilar-Rios, A.Montoya and I.Schifter, J.Sol-Gel Sci.Technol., 8, 107 (1997) prepared mesoporous aluminate materials with high specific surface area by sol-gel method, but these mesopores are aluminate nanometers prepared by sol-gel method. The accumulation pores formed by the accumulation of particles are not structural pores in the true sense; and because expensive metal alkoxides are used as the reaction starting material, the cost of the entire preparation process is high, and organic substances such as alcohols are also released during the calcination process , which makes the calcination process more dangerous, requires corresponding protective measures, and is not friendly to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Methanol and deionized water are configured 75ml hydrothermal solution by volume ratio 1:1, then take 0.075 mole zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 0.15 mol aluminum nitrate (Al(NO 3 ) 3 9H 2 (2) and 2.25 moles of urea were dissolved in the above hydrothermal solution, and transferred to a hydrothermal kettle for hydrothermal reaction at 160°C for 24 hours, and finally the product was separated and washed with water and alcohol, and dried at 70°C for 12 hours to obtain the obtained product Need materials. The pore size distribution of the material is dominated by micropores, the most probable pore size is 0.9nm, and the specific surface area is 320m 2 g -1 .

Embodiment 2

[0017] Ethanol and deionized water are configured 75ml hydrothermal solution by volume ratio 1:3, then take 0.05 mole of zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 0.1 mole aluminum nitrate (Al(NO 3 ) 3 9H 2 O) and 0.6 moles of urea were dissolved in the above-mentioned hydrothermal solution, and transferred to a hydrothermal kettle for hydrothermal reaction at 180°C for 12 hours, and finally the product was separated and washed with water and alcohol, and dried at 90°C for 10 hours to obtain the obtained product Need materials. The pore size distribution of the material exists in both micropore and mesopore range, the most probable pore size is 4.3nm, and the specific surface area is 230m 2 g -1 .

Embodiment 3

[0019] Ethanol and deionized water are configured 75ml hydrothermal solution by volume ratio 1:1, then take 0.05 mole of zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 0.1 mole aluminum nitrate (Al(NO 3 ) 3 9H 2 O) and 1 mole of urea were dissolved in the above hydrothermal solution, and transferred to a hydrothermal kettle for hydrothermal reaction at 180°C for 12 hours, and finally the product was separated and washed with water and alcohol, and dried at 80°C for 12 hours to obtain the obtained Need materials. The pore size distribution of the material exists in both micropore and mesopore range, the most probable pore size is 3.8nm, and the specific surface area is 240m 2 g -1 .

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Abstract

The invention discloses a preparing method of high-specific surface area micro / dielectric hole aluminate in the inorganic chemical synthetic domain, which comprises the following steps: adopting bivalent metal salt, aluminium salt, urea, deionized water and alcohol to allocate water heat solution; placing solution in the water hot autoclave; stewing to do water hot reaction; separating product; washing through alcohol; drying to obtain the product; making the specific area over 200m2g-1; adjusting the aperture distribution and specific surface area through controlling reacting condition.

Description

technical field [0001] The invention belongs to the field of inorganic chemical synthesis, and in particular provides a method for preparing micro / mesoporous aluminate with high specific surface area in one step. technical background [0002] According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), porous materials can be divided into three categories according to their pore size: micropores less than 2nm, mesoporous 2-50nm, and macropores greater than 50nm. As an effective solid catalyst, microporous zeolite molecular sieve has been widely used in the fields of petroleum refining, fine chemical industry and adsorption separation. Since 1992, researchers from Mobil Corporation of the United States synthesized M41S molecular sieve materials with uniform pore size distribution by using supramolecular self-assembly of surfactants in a mild hydrothermal system. It exceeds the limit of 1.2nm, and has the characteristics of adjustable regular ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/00C01B37/00
Inventor 李峰邹鲁项顼
Owner BEIJING UNIV OF CHEM TECH