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Method for preparing heteropoly acid/ordered mesic porous silicon oxide catalyst, and its application

A technology of mesoporous silicon oxide and heteropolyacid, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problems of difficult recovery, low activity, and emission pollution and other issues to achieve the effect of ensuring high activity, high catalytic activity and easy recycling

Inactive Publication Date: 2007-04-18
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, catalysts for oxidative desulfurization include formic acid, acetic acid, and heteropolyacids. Although these catalysts have high catalytic activity, they are difficult to recycle and easy to cause pollution when discharged.
Many solid catalysts such as TS-1, Mo / Al 2 o 3 etc. are also used in oxidative desulfurization catalysts, and their activity is relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of Heteropolyacid / Ordered Mesoporous Silica Catalysts:

[0021] Dissolve 0.82 g of phosphotungstic acid in a mixed solution of 20 g of absolute ethanol and 2.1 g of distilled water, then add 9.50 g of ethyl orthosilicate, and stir magnetically for 1 hour at room temperature to obtain mixed solution A. Then, 3.45 g of polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (P123) was dissolved in a mixed solution of 25 g of absolute ethanol and 2.1 g of distilled water to obtain mixed solution B. Then the mixed solution B was slowly poured into the previously stirred mixed solution A; the magnetic stirring was continued for 1 hour to obtain a uniform sol. Finally, the obtained sol was poured into a petri dish and stored at 40°C for 7 days; after pulverization, it was calcined at 400°C for 1 hour under nitrogen conditions, and then calcined at the same temperature for 1 day under air conditions to obtain phosphotungstic acid with a mass percentage ...

Embodiment 2

[0025] Preparation of Heteropolyacid / Ordered Mesoporous Silica Catalysts:

[0026] Dissolve 0.80 g of phosphomolybdic acid in a mixed solution of 20 g of absolute ethanol and 2.1 g of distilled water, then add 9.50 g of ethyl orthosilicate, and stir magnetically for 1 hour at room temperature to obtain mixed solution A. Then, 3.45 g of polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (P123) was dissolved in a mixed solution of 25.0 g of absolute ethanol and 2.1 g of distilled water to obtain mixed solution B. Then the mixed solution B was slowly poured into the previously stirred mixed solution A; the magnetic stirring was continued for 1 hour to obtain a uniform sol. Finally, the obtained sol was poured into a petri dish and stored at 40°C for 7 days; after pulverization, it was calcined at 400°C for 1 hour under nitrogen conditions, and then calcined for 1 day under the same temperature air condition, that is, the mass percentage of phosphomolybdic acid wa...

Embodiment 3

[0030] The heteropolyacid / ordered mesoporous silica catalyst in Example 1 was recycled eight times before use.

[0031]0.20g of heteropolyacid / ordered mesoporous silica catalyst was added to 20ml of petroleum ether solution of dibenzothiophene containing 500μg / g sulfur, then 20ml of acetonitrile was added as the extraction phase, and 276μL (volume) of 30% hydrogen peroxide was added at the same time. , so that the O / S molar ratio is 12:1. The final mixture was stirred at 60 °C for 3 h. , after the reaction, the oil is separated by filtration (the catalyst is removed by filtration), and the sample of the upper layer is obtained; the catalyst is recovered and washed with acetonitrile. The samples were analyzed by liquid chromatography (Aglient 6998N) to determine the residual sulfur content. The sulfur content of dibenzothiophene after the reaction was 6 μg / g, that is, the conversion rate of dibenzothiophene was 98.8%.

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Abstract

A heteropoly acid / ordered meso-porous silicon oxide catalyst used for removing the S-contained benzothiophenium compounds from the fractional oil of petroleum is prepared through such steps as dissolving heteropoly acid in the mixture of absolute alcohol and distilled water, adding ethyl n-silicate, magnetic stirring to obtain solution A, dissolving the polyoxyethene-polyoxypropene-polyoxyethene triblock copolymer in the mixture of absolute alcohol and distilled water to obtain solution B, slowly adding B to A, magnetic stirring to obtain sol, culturing it at 38-42 deg.C for 6-8 days, pulverizing, and calcining in N2.

Description

technical field [0001] The invention belongs to the technical field of petroleum processing and petrochemical industry, and in particular relates to a preparation method of a heteropolyacid / ordered mesoporous silica catalyst used for the oxidative removal of benzothiophene sulfur-containing compounds in petroleum distillates, and a heteropolyacid / ordered mesoporous silica catalyst. Application of polyacid / ordered mesoporous silica catalysts. Background technique [0002] In recent years, the tendency of crude oil to deteriorate worldwide has become increasingly obvious, and the content of sulfur, nitrogen and aromatic hydrocarbons in petroleum products has been increasing, and the contradiction between the increasingly strict environmental protection requirements and this reality has become more and more acute. More than one third of my country's petroleum products, especially diesel products, are produced by catalytic cracking processes. With the wide application of heavy ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188B01J23/24C10G45/04
Inventor 雷家珩颜学敏郭丽萍刘丹童辉
Owner WUHAN UNIV OF TECH
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