Palladium nanoparticle catalyst and preparation method as well as application thereof

A nanoparticle and metal nanoparticle technology, which is applied in the field of palladium nanoparticle catalyst preparation, can solve the problems that N atoms cannot combine with metal ions, affect the application, and lose dendritic compounds, so as to achieve recycling without pollution and good stability , the effect that is not easy to lose

Inactive Publication Date: 2010-11-03
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, under neutral conditions, the polyamine amine dendrimers with amino groups are easily combined with Pd 2+ When the noble metal ions are combined, the N atoms inside the dendron cannot be combined with the metal ion. After reduction, the metal element can only be reunited at the end of the dendritic compound, so that the dendritic compound loses the role of template and "anchor point", and this situation The shape and size of nanoparticles formed under the condition are uncontrollable, which affects its application

Method used

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  • Palladium nanoparticle catalyst and preparation method as well as application thereof
  • Palladium nanoparticle catalyst and preparation method as well as application thereof
  • Palladium nanoparticle catalyst and preparation method as well as application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Using the prepared catalyst to catalyze the microwave-assisted Suzuki coupling reaction of iodobenzene and phenylboronic acid

[0025] Under nitrogen protection, 0.8gK 3 PO 4 , 0.005g catalyst (0.5mol%), 0.128g phenylboronic acid (1.05mmol) are added in the 20ml microwave reaction flask that has 1.8ml deionized water, 1.2ml ethanol, wait to disperse evenly, add iodobenzene 1mmol, put into microwave after sealing In the reactor, react at 100°C for 30 minutes. After the reaction is finished, the organic phase is extracted with ethyl acetate, the inorganic water phase containing the catalyst powder is centrifuged, washed three times with water and washed twice with ethanol, and the catalyst is recovered by heating. The organic phase was extracted with saturated brine, and then dried over anhydrous sodium sulfate. After vacuum distillation, the product to be tested was obtained. The yield was measured by the external standard method in gas chromatography, and...

Embodiment 2

[0027] Example 2: Using the prepared catalyst to catalyze the microwave-assisted Suzuki reaction of iodobenzene and p-tolylboronic acid

[0028] Under nitrogen protection, 0.8gK 3 PO 4 , 0.005g of catalyst (0.5mol%), 1.05mmol of p-toluene boric acid 1.05mmol were added in a 20ml microwave reaction flask with 1.8ml of deionized water and 1.2ml of ethanol. In a microwave reactor, react at 100°C for 30 minutes.

[0029] After the reaction is finished, the organic phase is extracted with ethyl acetate, the inorganic water phase containing the catalyst powder is centrifuged, washed three times with water and washed twice with ethanol, and the catalyst is recovered by heating. The organic phase was extracted here with saturated brine and then dried over anhydrous sodium sulfate. After vacuum distillation, the product to be tested was obtained. The yield was measured by the external standard method in gas chromatography, and the yield was 91%.

Embodiment 3

[0030] Example 3: Using the obtained catalyst to catalyze the microwave-assisted Suzuki reaction of iodobenzene and p-methoxybenzeneboronic acid

[0031] Under nitrogen protection, 0.8gK 3 PO 4 , 0.005g catalyst (0.5mol%), 1.05mmol p-methoxyphenylboronic acid 1.05mmol are added in the 20ml microwave reaction bottle that has 1.8ml deionized water, 1.2ml ethanol, wait to disperse evenly, add iodobenzene 1mmol, seal and put Put it into a microwave reactor and react at 100°C for 30min.

[0032] After the reaction is finished, the organic phase is extracted with ethyl acetate, the inorganic water phase containing the catalyst powder is centrifuged, washed three times with water and washed twice with ethanol, and the catalyst is recovered by heating. The organic phase was extracted here with saturated brine and then dried over anhydrous sodium sulfate. After vacuum distillation, the product to be tested was obtained. The yield was measured by the external standard method in gas ...

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Abstract

The invention relates to a palladium nanoparticle catalyst and a preparation method as well as an application thereof. The preparation method comprises the following steps: controlling the pH of the reaction environment to be equal to 2; combining metal ions of different concentrations with inner N of branches; and finally, reducing the metal ions by utilizing NaBH4 to generate a metal Pd nanoparticle catalyst with different diameters (1-3nm) of particles. The catalyst has good catalytic effect on the Suzuki reaction aided by microwaves. The method has the characteristics of simple process, convenient operation, controllable shape, good application effect and the like.

Description

technical field [0001] The present invention relates to a kind of preparation method of palladium nano particle catalyst, specifically, utilize the internal cavity of the dendritic compound grafted in the mesoporous SBA-15, prepare the nano catalyst that can be used for catalyzing the microwave-assisted Suzuki reaction, It belongs to the field of catalyst materials. Background technique [0002] Coupling reactions such as Suzuki have always been an extremely important intermediate reaction process in organic reactions. At present, this kind of reaction and its related reactions have been widely used in the preparation of new pharmaceutical materials and other methods, and the application methods are constantly being innovated, which has far-reaching application value. [0003] The catalysts that catalyze the suzuki reaction are mainly catalysts represented by noble metals such as palladium, and general catalysts can be divided into homogeneous catalysts and heterogeneous ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J31/06B01J37/16C07C15/14C07C1/32C07C43/205C07C41/30
Inventor 曹荣郑兆亮
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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