Preparation method of heteropoly acid / alumina mesoporous composite material

A composite material and a technology for heteropolyacids, which are applied in the field of preparation of heteropolyacid/alumina mesoporous composite materials, can solve the problems of structural destruction of heteropolyacids, reduced catalytic activity, incompatibility, etc., and achieve easy separation, recovery, selection, etc. good effect

Inactive Publication Date: 2011-11-23
YANGTZE UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the composite method of heteropolyacid and mesoporous alumina is still dominated by the traditional impregnation method. Due to the strong surface acidity of mesoporous alumina, the structure of heteropolyacid is often destroyed, which leads to its catalytic The activity is reduced and cannot meet the needs of practical applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 4.09g of aluminum isopropoxide in 30g of absolute ethanol solution, add 2.6g of nitric acid to adjust the pH value, add 0.28g of phosphotungstic acid after the aluminum isopropoxide is completely dissolved, and stir at room temperature for 6 hours to obtain a solution (1) ; Then 1.85g polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (P123) was dissolved in 10g absolute ethanol to obtain solution (2); then solution (2) was slowly poured into solution (1 ); continue to stir for 5 hours to obtain a uniform sol; finally pour the obtained sol into a petri dish and store it at 60°C for 48 hours to obtain a light yellow film sample; after grinding the sample, calcinate it at 420°C for 3 days to obtain phosphorus-containing tungsten Acidic heteropolyacid / alumina mesoporous composites. The heteropoly acid / alumina mesoporous composite has an average pore diameter of 3.2nm and a specific surface area of ​​160m 2 / g.

Embodiment 2

[0030] Dissolve 2.0 g of aluminum isopropoxide in 16 g of absolute ethanol solution, add 1.5 g of nitric acid to adjust the pH value, add 0.15 g of phosphomolybdic acid after the aluminum isopropoxide is completely dissolved, and stir for 5 hours at room temperature to obtain solution (1) ; Then 0.96g polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (P123) was dissolved in 5g absolute ethanol to obtain solution (2); then solution (2) was slowly poured into solution (1 ); continue to stir for 5 hours to obtain a uniform sol; finally pour the obtained sol into a petri dish, store at 60°C for 48h to obtain a light yellow film sample; after grinding the sample, calcined at 420°C for 3 days to obtain phosphorus-containing molybdenum Acidic heteropolyacid / alumina mesoporous composites. The heteropoly acid / alumina mesoporous composite has an average pore diameter of 3.5nm and a specific surface area of ​​152m 2 / g.

Embodiment 3

[0032] Dissolve 8.12g of aluminum isopropoxide in 60g of absolute ethanol solution, add 5.4g of nitric acid to adjust the pH value, add 0.55g of silicotungstic acid after the aluminum isopropoxide is completely dissolved, and stir at room temperature for 6 hours to obtain a solution (1) ; Then 4.0g polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (P123) was dissolved in 20g absolute ethanol to obtain solution (2); then solution (2) was slowly poured into solution (1 ); continue to stir for 6 hours to obtain a uniform sol; finally pour the obtained sol into a petri dish and store at 60°C for 36 hours to obtain a light yellow film sample; after grinding the sample, calcined at 410°C for 3 days to obtain silicon-containing tungsten Acidic heteropolyacid / alumina mesoporous composites. The heteropoly acid / alumina mesoporous composite has an average pore diameter of 3.0nm and a specific surface area of ​​162m 2 / g.

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Abstract

The invention relates to a preparation method of a heteropoly acid / alumina mesoporous composite material, which is characterized in that the method comprises the following steps: dissolving aluminum isopropoxide in anhydrous alcohol, adjusting the pH value by nitric acid, adding heteropoly acid; stirring at room temperature for 4-8 hours to obtain a solution (1); dissolving a polyoxyethylene- polyoxypropylene-polyoxyethylene triblock copolymer (P123) into anhydrous alcohol to obtain a solution (2); slowly adding the solution (2) into the solution (1), stirring for 4-8 hours to obtain a uniform sol; pouring the sol into a culture dish, preserving the culture dish at 60 DEG C for 36-58 hours to obtain a light yellow film sample, grinding the sample, calcining at 400-420 DEG C for 2-3 days to obtain the heteropoly acid / alumina mesoporous composite material. The invention can effectively protect the heteropoly acid structure from being destroyed, and the material prepared by the invention has the characteristics of high activity, good selectivity, easy separation and recovery, and recyclability, and can be used as a catalyst for fuel oil deep oxidation and desulphurization in the petroleum chemical industry field.

Description

Technical field: [0001] The invention relates to a preparation method of a heteropolyacid / alumina mesoporous composite material, and belongs to the technical field of preparation of petrochemical fuel oil deep oxidation desulfurization catalysts. Background technique: [0002] Sulfur contained in fuel oil is an important source of urban air pollution. With the continuous improvement of people's requirements for environmental protection in the 21st century, countries around the world have enacted strict regulations on the sulfur content in fuel oil. Traditional hydrodesulfurization technology has very limited ability to remove high content of benzothiophene, dibenzothiophene and their derivatives in fuel oil, mainly because these sulfide molecules have high steric hindrance and are difficult to access to catalytic active center. In order to meet the requirements of low sulfur, high temperature, high pressure, larger reaction vessel and more active catalyst are required, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188B01J27/19B01J23/30B01J23/28B01J35/10C10G27/12
Inventor 颜学敏梅平苏高申熊麟
Owner YANGTZE UNIVERSITY
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