Mesoporous carbon supported N-heterocyclic carbene-palladium catalyst as well as preparation and application thereof

A nitrogen heterocyclic carbene, palladium catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the loss of palladium and affect the reuse of supported catalysts performance and other issues, to achieve the effect of preventing loss, excellent reuse performance, and improving catalytic activity

Inactive Publication Date: 2015-04-15
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It must be pointed out that although the supported nitrogen-heterocyclic carbene palladium catalyst prepared with the above-mentioned carrier has good catalytic activity, palladium often loses during the catalytic process, which affects the reusable performance of the supported catalyst to a large extent.

Method used

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  • Mesoporous carbon supported N-heterocyclic carbene-palladium catalyst as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 2.0 g of SBA-15 into a mixed solution of 10 g of deionized water, 2.50 g of sucrose and 0.28 g of concentrated sulfuric acid, place the above mixture in an oven and heat it at 373K for 6 hours, then raise the temperature to 433K and heat it for 6 hours to obtain a brown solid; grind Then add a mixed solution of 10 g of deionized water, 1.60 g of sucrose and 0.18 g of concentrated sulfuric acid, and repeat the above heating steps. After the obtained product was carbonized at a constant temperature of 823K for 5 hours in an argon atmosphere, the cooled black powder was added to 100 g of HF solution (10% by mass) to remove the ordered mesoporous silicon template SBA-15, washed several times with distilled water and dried at 393K. The ordered mesoporous carbon material CMK–3 can be obtained. Add 2g of concentrated nitric acid (68% by mass) to the bottom of the polytetrafluoroethylene inner liner of a 100mL autoclave, place a polytetrafluoroethylene beaker containing 0.3...

Embodiment 2

[0030]Add 0.5 g of the hydroxylated mesoporous carbon to 100 g of toluene solution containing trimethoxychloropropane, wherein the mass percentage of the toluene solution of trimethoxychloropropane is 2.0%, ultrasonically vibrate for 120 min, and at a temperature of 80 The reaction was stirred at ℃ for 720 minutes, cooled to room temperature, and the product was centrifuged, washed with 10 g of ethanol and 10 g of distilled water in turn, and dried in vacuum to obtain a black powder, which is chloropropyl silicon mesoporous carbon. Add 0.4 g of the mesoporous carbon of chloropropyl silicon to 100 g of imidazole-containing toluene solution, wherein the mass percentage of imidazole in toluene solution is 5.0%, ultrasonically oscillate for 120 min, and stir the reaction at a temperature of 80 ° C After cooling to room temperature for 720 min, the product was centrifuged and washed successively with 10 g of ethanol and 10 g of distilled water until the eluent was neutral; after fre...

Embodiment 3

[0032] Add 0.5 g of the hydroxylated mesoporous carbon to 100 g of toluene solution containing trimethoxychloropropane, wherein the mass percentage of the toluene solution of trimethoxychloropropane is 2.0%, ultrasonically vibrate for 120 min, and at a temperature of 80 The reaction was stirred at ℃ for 720 minutes, cooled to room temperature, and the product was centrifuged, washed with 10 g of ethanol and 10 g of distilled water in turn, and dried in vacuum to obtain a black powder, which is chloropropyl silicon mesoporous carbon. Add 0.4g of the mesoporous carbon of chloropropyl silicon to 100g of toluene solution containing 1-methylimidazole, wherein the mass percentage of the toluene solution of 1-methylimidazole is 5.0%, ultrasonically vibrate for 120min, at temperature Stir and react at 80°C for 720min, cool to room temperature, and centrifuge the product, then wash with 10g of ethanol and 10g of distilled water until the eluent is neutral; after freeze-drying, the black...

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Abstract

The invention discloses a mesoporous carbon supported N-heterocyclic carbene-palladium catalyst as well as a preparation method and application thereof. The catalyst carrier is hydroxylated mesoporous carbon; the ligand is N-heterocyclic carbine; the active ingredient is palladium chloride; the load capacity of the palladium in the active ingredient is 5.0-10.0% of the total mass of the catalyst; the surface hydroxyl group content of the hydroxylated mesoporous carbon is 1.9-2.2 mmol / g; the BET specific surface area of the hydroxylated mesoporous carbon is 700-1000m<2> / g; the BJH pore diameter is 5-7 nm; the BJH pore volume is 0.8-1.8 ml / g. According to the mesoporous carbon supported N-heterocyclic carbene-palladium catalyst, the palladium can be prevented from loss in the catalytic process; the mesoporous carbon has an ordered mesoporous structure, so that the surface dispersing performance of the palladium nano-particles can be improved to prevent the palladium from gathering in the catalytic process and improve the catalytic activity of the supported catalyst. The mesoporous carbon supported N-heterocyclic carbene-palladium catalyst has relatively high catalytic activity and relatively good reusability.

Description

field of invention [0001] The invention relates to a mesoporous carbon-supported nitrogen heterocyclic carbene palladium catalyst, a preparation method and an application. Background technique [0002] Nitrocyclic carbene palladium complexes are widely used in palladium-catalyzed C-C coupling reactions due to their stable physical and chemical properties and strong catalytic activity. For example, Wang Ruihu, Fujian Institute of Material Structure, Chinese Academy of Sciences, etc. developed a pH-responsive nitrogen heterocyclic carbene palladium complex. The catalyst can make the Suzuki reaction of aryl chlorides proceed smoothly in pure water medium. Godoy synthesized a series of sulfonated nitrogen-heterocyclic carbene palladium complexes, and the catalysts can activate aryl chlorides in the presence of phase-transfer catalyst tetrabutylammonium bromide. However, although nitrogen-heterocyclic carbene palladium complexes have made significant progress in C-C coupling re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07B37/04
Inventor 袁定重张庆华张志宾陈龙熊鑫元利刚杨梦梅熊文文廖世军蒋烨佳陈洪剑
Owner EAST CHINA UNIV OF TECH
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