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A kind of keggin type heteropolyacid-silicon oxide catalyst with mesopore structure and preparation method thereof

A silicon oxide and catalyst technology, applied in the field of catalysis, can solve the problems of poor reusability, easy dissolution and removal of active component heteropolyacids, etc., and achieve the effects of easy separation and recovery, easy industrial production, and high activity

Inactive Publication Date: 2016-01-20
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a Keggin type heteropolyacid-silicon oxide catalyst with a mesoporous structure and a preparation method thereof, which can solve the problem that the active component heteropolyacid in the current supported catalyst is easy to dissolve and desorb in the reaction system, and the reusability is poor. question

Method used

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  • A kind of keggin type heteropolyacid-silicon oxide catalyst with mesopore structure and preparation method thereof
  • A kind of keggin type heteropolyacid-silicon oxide catalyst with mesopore structure and preparation method thereof
  • A kind of keggin type heteropolyacid-silicon oxide catalyst with mesopore structure and preparation method thereof

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Embodiment 1

[0030] 5wt% of the mesoporous structure (the weight percent of phosphotungstic heteropolyacid in the catalyst, the same below) Keggin type heteropolyacid-silicon oxide catalyst, the preparation steps are as follows:

[0031] Dissolve 2g of P123 in 70mL of hydrochloric acid solution (hydrochloric acid: water volume ratio is 1:6, the same below) at 40°C, dissolve 0.0649g of phosphotungstic heteropoly acid in 10mL of deionized water, and slowly pour the phosphotungstic acid solution into P123 solution, and added 4.6mL tetraethyl orthosilicate dropwise, stirred at a constant temperature for 24 hours, then stopped stirring, raised the temperature to 90°C to maintain a constant temperature, and stood it under normal pressure for 24 hours, suction filtered and washed with deionized water, and the obtained white filter cake was placed in After drying at room temperature, grinding, and roasting at 400°C for 5 hours, a 5wt% phosphotungstic heteropolyacid-silicon oxide catalyst was obtain...

Embodiment 2

[0033] 5wt% of the mesoporous structure (the weight percent of silicotungstic heteropolyacid in the catalyst, the same below) Keggin type silicotungstic heteropolyacid-silica catalyst, the specific preparation steps are as follows:

[0034] Dissolve 2g of P123 in 70mL of hydrochloric acid solution (1:6) at 40°C, dissolve 0.0649g of silicotungstic acid in 10mL of deionized water, slowly pour the silicotungstic acid solution into the P123 solution, and add 4.6mL of orthosilicic acid dropwise Ethyl ester, stirred at constant temperature for 24 hours, then stopped the stirring, raised the temperature to 90°C to maintain a constant temperature, stood still at normal pressure for 24 hours, filtered with suction, washed with deionized water, dried the obtained white filter cake at room temperature, and ground it under the condition of 400°C Calcined for 5 hours to obtain 5wt% silicotungstic heteropolyacid-silica catalyst with an average pore diameter of 4.79nm and a specific surface a...

Embodiment 3

[0036] The 10wt% phosphotungstic heteropoly acid-silicon oxide catalyst with mesoporous structure, the specific preparation steps are as follows:

[0037] Dissolve 2g P123 in 70mL hydrochloric acid solution (1:6) at 40°C, dissolve 0.1376g phosphotungstic acid in 10mL deionized water, slowly pour the phosphotungstic acid solution into the P123 solution, and add 4.6mL orthosilicate dropwise Ethyl ester, stirred at constant temperature for 24 hours, then stopped the stirring, raised the temperature to 90°C to maintain a constant temperature, stood still at normal pressure for 24 hours, filtered with suction, washed with deionized water, dried the obtained white filter cake at room temperature, and ground it under the condition of 400°C Calcined for 5 hours to obtain 10wt% phosphotungstic heteropolyacid-silica catalyst with an average pore diameter of 5.11nm and a specific surface area of ​​971m 2 / g.

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Abstract

The invention belongs to the catalysis technical field, and particularly relates to a Keggin type heteropoly acid-silicon oxide catalyst of a mesopore structure and a preparation method of the catalyst. The average pore diameter of the catalyst is 4.50-5.55nm, the specific surface area is 728-971m<2> / g, and the content of the heteropoly acid is 1-35% which is calculated in percentage by weight. The heteropoly acid which is loaded by the catapyst is not easy to dissolve, and has features of high activity, good selectivity, easy separation and recovery, repeated use, and easy implement of the industrialized production. The catalyst can be used for the esterification and oxidation reaction system of relatively large molecular weight reaction substances.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a Keggin type heteropolyacid-silicon oxide catalyst with mesoporous structure and a preparation method thereof. Background technique [0002] As a new type of catalytic material, heteropolyacid has strong acidity, is relatively stable, non-toxic and easy to handle, and does not produce side reactions such as sulfidation, chlorination and nitration, and has shown broad application prospects in the fields of oil refining and chemical industry. However, the specific surface area of ​​heteropoly acids is small (<10m 2 / g), as a solid catalyst, it needs to be supported to increase its specific surface area, so that the active components can be fully utilized. However, the existing preparation methods of silica-supported heteropolyacid catalysts often have defects such as low yield, complicated process, unfriendly environment, and low catalytic efficiency, and the act...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/16B01J31/18B01J35/10
Inventor 郑修成张晓丽陈雅陈茜关新新
Owner ZHENGZHOU UNIV