Sulfydryl functionalized ordered mesoporous silicon-immobilized Au heterogeneous catalyst and preparation method and application thereof

A heterogeneous catalyst and functionalization technology, applied in the direction of physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve heavy metal pollution, and homogeneous catalysts are difficult to reuse , Improve the reaction cost and other issues, to achieve the effect of smooth channels, uniform distribution of active sites, and realization of recycling

Inactive Publication Date: 2010-07-28
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional catalysts for alkyne hydration reactions are mainly mercury. Although a variety of organic Au complexes have been developed recently to replace mercury with strong toxicity, homogeneous catalysts have always been difficult to reuse, easy to cause heavy metal pollution and increase the reaction rate. Cost and other issues

Method used

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  • Sulfydryl functionalized ordered mesoporous silicon-immobilized Au heterogeneous catalyst and preparation method and application thereof
  • Sulfydryl functionalized ordered mesoporous silicon-immobilized Au heterogeneous catalyst and preparation method and application thereof
  • Sulfydryl functionalized ordered mesoporous silicon-immobilized Au heterogeneous catalyst and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A preparation method of Au heterogeneous catalyst supported by ordered mesoporous silicon with thiol functionalization, comprising the following steps:

[0036] 1) 1.0g P123 (EO 20 PO 70 EO 20 ) (0.17mmol), 8.0g H 2 O and 31mL 2M HCl solution were mixed, stirred at 40°C for 3h in the jacket, and then 9.5mmol tetraethyl orthosilicate (TEOS) was added. Base mercaptan (0.5mmol), continue to stir for 24h, age at 100°C for 24h, filter, wash, and vacuum dry to obtain a white solid powder;

[0037] 2) Grind the above materials with an agate mortar, and finally mix them with HCl / C 2 h 5 OH is extracted, and the mass volume ratio of solid and liquid is 1g: 1000mL; In the described mixed solution of hydrochloric acid and ethanol, the content of hydrochloric acid is 1.0mol / L, and the content of ethanol is 750g / L. The obtained product is ordered mesoporous silicon functionalized with mercapto groups, represented by SH-SBA-15. The small angle XRD picture is as follows figure...

Embodiment 2

[0044] A preparation method of Au heterogeneous catalyst supported by ordered mesoporous silicon with thiol functionalization, comprising the following steps:

[0045] 1) 0.9g P123 (EO 20 PO 70 EO20 ) (0.16mmol), 8.0g H 2 O and 31mL of 2M HCl solution were mixed, stirred at 40°C for 3h in the jacket, and then added (9.6mmol) orthoethyl silicate (TEOS). After 90min of prepolymerization of TEOS, 3-trimethoxysilane Propyl mercaptan (0.4mmol), continued to stir for 22h, aged at 100°C for 24h, filtered, washed, and vacuum dried to obtain a white solid powder;

[0046] 2) Grind the above materials with an agate mortar, and finally mix them with HCl / C 2 h 5 OH for extraction to obtain ordered mesoporous silicon functionalized with mercapto groups; represented by SH-SBA-15. The mass volume ratio of solid and liquid is 1g:900mL; in the mixed solution of hydrochloric acid and ethanol, the content of hydrochloric acid is 1.1mol / L, and the content of ethanol is 750g / L.

[0047] 3) A...

Embodiment 3

[0049] A preparation method of Au heterogeneous catalyst supported by ordered mesoporous silicon with thiol functionalization, comprising the following steps:

[0050] 1) 1.1g P123 (EO 20 PO 70 EO 20 ) (0.19mmol), 9.0g H 2 O and 31mL of 2M HCl solution were mixed, stirred at 40°C for 3h in a jacketed jacket, and then (9.7mmol) tetraethyl orthosilicate (TEOS) was added. After TEOS was prepolymerized for 90min, 3-trimethoxysilane was added n-Propylmercaptan (0.3mmol), continue to stir for 26h, age at 100°C for 24h, filter, wash, and vacuum dry to obtain a white solid powder;

[0051] 2) Grind the above materials with an agate mortar, and finally mix them with HCl / C 2 h 5 OH for extraction to obtain ordered mesoporous silicon functionalized with mercapto groups; represented by SH-SBA-15. The mass volume ratio of solid and liquid is 1g:800mL; in the mixed solution of hydrochloric acid and ethanol, the content of hydrochloric acid is 0.8mol / L, and the content of ethanol is 65...

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Abstract

The invention relates to sulfydryl functionalized ordered mesoporous silicon-immobilize Au heterogeneous catalyst and a preparation method and application thereof. The preparation method is as follows: mixing surfactant, strong acid, water, ethyl orthosilicate and sulfhydryl silane under heating condition, continuously stirring the reactant mixture, filtering the reactant mixture to get white solid, and sequentially washing and drying the white solid to get a sulfydryl functionalized ordered mesoporous silicon carrier; mixing the carrier with ethanol and HAuCl4 solution, stirring for 24h under room temperature, pump filtering and washing the mixture, and vacuum drying overnight. In this way, the ordered mesoporous sulfydryl functionalized SBA-15-immobilize Au heterogeneous catalyst can be formed. The preparation process is simple and the heterogeneous catalyst prepared through the method has efficient and long-lasting catalytic activity, can improve the reaction speed, reduce the production cost and improve the quality of the product, and can be recycled for use, thereby reducing environment pollution.

Description

technical field [0001] The invention relates to a preparation process and application of an ordered mesoporous heterogeneous catalyst, in particular to a preparation method of an ordered mesoporous mercapto-functionalized SBA-15 immobilized Au heterogeneous catalyst and its application in an aqueous medium Applications in clean alkyne hydration reactions. Background technique [0002] In recent years, the use of water instead of organic solvents for organic synthesis has become an important branch of green chemistry. Hydration of alkynes is an important class of organic reactions, and the products obtained are important intermediates in organic synthesis. The traditional catalysts for alkyne hydration reactions are mainly mercury. Although a variety of organic Au complexes have been developed recently to replace mercury with strong toxicity, homogeneous catalysts have always been difficult to reuse, easy to cause heavy metal pollution and increase the reaction rate. cost a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/52C07C45/26C07C49/04C07C49/78C07C49/84C07C49/76C07C49/807C07C49/80
Inventor 朱凤霞李和兴张昉
Owner SHANGHAI NORMAL UNIVERSITY
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