Method for preparing dispersed palladium nanoparticle catalyst with controllable appearance by using cucurbit[6]uril (CB[6])

A technology of palladium nanoparticles and six-membered melon rings, which is applied in the field of preparation of palladium nanoparticle catalysts, can solve problems such as the research on protective reagents for metal nanoparticles, the inability to prevent the aggregation of nanoparticles, and the reduction of catalytic activity of catalysts. , to achieve the effect of high cycle times, convenient operation and simple method

Active Publication Date: 2011-10-05
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Surfactant functional groups can form covalent interactions with metal nanoparticles, limiting and reducing their catalytic activity
Although the internal cavity of dendrimers can effectively inhibit the agglomeration of nanoparticles, it also reduces the catalytic activity of the catalyst to a large extent.
However,

Method used

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  • Method for preparing dispersed palladium nanoparticle catalyst with controllable appearance by using cucurbit[6]uril (CB[6])
  • Method for preparing dispersed palladium nanoparticle catalyst with controllable appearance by using cucurbit[6]uril (CB[6])
  • Method for preparing dispersed palladium nanoparticle catalyst with controllable appearance by using cucurbit[6]uril (CB[6])

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: utilize CB[6] to prepare spherical palladium nanoparticles as dispersant

[0028] 0.4g CB[6], 0.035g PdCl 2 (molar ratio 2:1) mixed with 20mL 50% ethanol aqueous solution, stirred for half an hour to obtain a uniform suspension; 0.076g NaBH 4 (2mmol, 10 times equivalent to PdCl 2 ) was dissolved in 20 mL of 50% ethanol aqueous solution and quickly added to the above suspension. The reaction was continued for 3 hours and then centrifuged, and the solid product was washed once with ethanol and water. After drying, the ethanol was redispersed, and the product was observed by a transmission electron microscope to obtain a monodisperse, approximately spherical palladium nanoparticle catalyst with a particle size of 3.3±0.1nm.

Embodiment 2

[0029] Embodiment 2: utilize CB[6] to prepare spherical palladium nanoparticles as dispersant

[0030] 0.2g CB[6], 0.035g PdCl 2 (molar ratio 1:1) mixed with 20mL 50% ethanol aqueous solution, stirred for half an hour to obtain a uniform suspension; 0.076g NaBH 4 (2mmol, 10 times equivalent to PdCl 2 ) was dissolved in 20 mL of 50% ethanol aqueous solution and quickly added to the above suspension. The reaction was continued for 3 hours and then centrifuged, and the solid product was washed once with ethanol and water. After drying, the ethanol is redispersed, and the product is spherical nanoparticles with a particle size of 3.3±0.2nm observed by a transmission electron microscope.

Embodiment 3

[0031] Example 3: Preparation of cubic palladium nanoparticles using CB[6] as a dispersant

[0032] 0.2g CB[6], 0.070g PdCl 2 (molar ratio 1:2) mixed with 20mL 50% ethanol aqueous solution, stirred for half an hour to obtain a uniform suspension; 0.152g NaBH 4 (4mmol, 10 times equivalent to PdCl 2 ) was dissolved in 20 mL of 50% ethanol aqueous solution and quickly added to the above suspension. The reaction was continued for 3 hours and then centrifuged, and the solid product was washed once with ethanol and water. After drying, ethanol was redispersed, and the product was cubic nanoparticles observed by transmission electron microscopy.

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Abstract

The invention provides a method for preparing a dispersed palladium nanoparticle catalyst with controllable appearance by using CB[6]. The present invention is characterized in that a mole ratio of CB[6] to a metallic precursor (PdCl2) is adjusted, the metal ion can be reduced by NaBH4, the dispersed and uniform (to 3.3nm) metal Pd nanoparticle catalyst with controllable appearance can be prepared under a mild condition. The catalyst has the advantages of high catalytic activity and stability, which can realize a high efficient catalysis to a coupling reaction of Suzuki in air, and the catalyst enables a repeated use. The method of the present invention has the characteristics of simple technology, convenient operation, controllable appearance and good application effect and the like.

Description

technical field [0001] The invention relates to a preparation method of a palladium nano particle catalyst whose shape is controlled by using a six-membered melon ring to disperse. The method utilizes the special structure and properties of the six-membered melon ring to effectively disperse nano-palladium particles to prepare a nano-catalyst that can be used for Suzuki reaction under mild conditions, and belongs to the field of catalyst materials. Background technique [0002] Suzuki coupling reaction has always been one of the most effective methods for the synthesis of biaryl compounds, and has been a research hotspot in catalytic chemistry and organic chemistry in recent years; Suzuki coupling reaction is also the preparation of many natural products and a large number of drug molecules and pesticides It must go through the reaction process and has far-reaching application value. [0003] Catalysts for the Suzuki reaction are mainly catalysts represented by noble metals...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J33/00B01J35/08B01J35/10C07C15/14C07C1/32
Inventor 曹荣曹敏纳
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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