Rotatable magnetic nano chain supported palladium nanoparticle catalyst and preparation method thereof

A magnetic nanochain and nanochain technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low recycling rate, easy agglomeration, difficult separation of catalysts, etc., to achieve growth strength Effect

Active Publication Date: 2019-08-23
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to avoid the deficiencies of the prior art: the problems of easy agglomeration of the noble metal palladium nanoparticle catalyst, difficult separation of the catalyst after the reaction, low recycling rate, etc., the present invention proposes a self-rotating magnetic nano chain loaded palladium nanoparticle catalyst and Its preparation method is to load palladium nanoparticles through the rotation of one-dimensional rattle-shaped magnetic nano-chains in an alternating magnetic field and the high specific surface area and porosity provided by the rattle-shaped structure, and use an external magnetic field to separate and recover the magnetic nano-chains. Solve the above-mentioned problems that palladium metal nanoparticle catalyst exists

Method used

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  • Rotatable magnetic nano chain supported palladium nanoparticle catalyst and preparation method thereof
  • Rotatable magnetic nano chain supported palladium nanoparticle catalyst and preparation method thereof
  • Rotatable magnetic nano chain supported palladium nanoparticle catalyst and preparation method thereof

Examples

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Effect test

Embodiment 1

[0039] Step 1. Preparation of core-shell Fe by distillation-precipitation polymerization induced by external magnetic field 3 o 4 @P(DVB-MAA) magnetic nanochain. Disperse 0.026g of magnetic microspheres, 0.072g of divinylbenzene and 0.271g of methacrylic acid in 80mL of acetonitrile, and then add 7.5mg of AIBN after ultrasonication for 1 hour. React for 1 hour, collect the product by magnetic separation, and wash the product 3 times with absolute ethanol and deionized water, respectively, to obtain the core-shell Fe 3 o 4 @P(DVB-MAA) magnetic nanochain.

[0040] Step 2, the obtained Fe 3 o 4 @P(DVB-MAA) magnetic nanochains were dispersed in a mixed solvent containing 50mL of absolute ethanol and 6.25mL of deionized water, and 2mL of ammonia water was added under mechanical stirring at 280r / min. After stirring for 1 hour, 0.15mL of TEOS was added in sequence React with 0.03mL of octadecyltrimethoxysilane overnight at room temperature, perform magnetic separation, wash wit...

Embodiment 2

[0044] Step 1. Preparation of core-shell Fe by distillation-precipitation polymerization induced by external magnetic field 3 o 4@P(DVB-MAA) magnetic nanochain. Disperse 0.022g of magnetic microspheres, 0.071g of divinylbenzene and 0.273g of methacrylic acid in 80mL of acetonitrile, and then add 7.5mg of AIBN after ultrasonication for 1 hour. After the dissolution is complete, transfer the mixed solution into a three-necked flask, and react in a water bath at 80°C After 1 hour, the product was collected by magnetic separation, and the product was washed 4 times with absolute ethanol and deionized water, respectively, to obtain the core-shell Fe 3 o 4 @P(DVB-MAA) magnetic nanochain.

[0045] Step 2, the obtained Fe 3 o 4 @P(DVB-MAA) magnetic nanochains were dispersed in a mixed solvent containing 50mL of absolute ethanol and 6.25mL of deionized water, and 2mL of ammonia water was added under mechanical stirring at 280r / min. After stirring for 1 hour, 0.15mL of TEOS was add...

Embodiment 3

[0049] Step 1. Preparation of core-shell Fe by distillation-precipitation polymerization induced by external magnetic field 3 o 4 @P(DVB-MAA) magnetic nanochain. Disperse 0.02g of magnetic microspheres, 0.07g of divinylbenzene and 0.27g of methacrylic acid in 80mL of acetonitrile, and then add 7.5mg of AIBN after ultrasonication for 1 hour. After the dissolution is complete, transfer the mixed solution into a three-necked flask, and react in a water bath at 80°C 1h, the product was collected by magnetic separation, and the product was washed 3 to 4 times with absolute ethanol and deionized water, respectively, to obtain the core-shell Fe 3 o 4 @P(DVB-MAA) magnetic nanochain.

[0050] Step 2, the obtained Fe 3 o 4 @P(DVB-MAA) magnetic nanochains were dispersed in a mixed solvent containing 50mL of absolute ethanol and 6.25mL of deionized water, and 2mL of ammonia water was added under mechanical stirring at 280r / min. After stirring for 1 hour, 0.15mL of TEOS was added in s...

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Abstract

The invention relates to a rotatable magnetic nano chain supported palladium nanoparticle catalyst and a preparation method thereof. The preparation method comprises the following steps: firstly, carrying out external magnetic field induced assembling so as to obtain a one-dimensional core-shell type Fe3O4@(DVB-MAA) nano chain; secondly, carrying out silica coating on the Fe3O4@(DVB-MAA) nano chain by using a simple sol-gel method, and preparing a bell-shaped Fe3O4@Void@mSiO2 magnetic nano chain through firing; and finally carrying out amino modification on the surface of the bell-shaped Fe3O4@Void@mSiO2 magnetic nano chain, supporting palladium ions on the magnetic nano chain under an intensive complexing function of amino and palladium ions (Pd<2+>), and reducing the supported palladiumions, thereby obtaining a one-dimensional magnetic hollow nano chain supported palladium nanoparticle catalyst. By adopting the catalyst, the problem that a noble metal, namely palladium nanoparticles, is hard to separate and liable to aggregate when being used as a catalyst, can be effectively solved.

Description

technical field [0001] The invention belongs to a noble metal palladium catalyst and a preparation method thereof, and relates to a palladium nanoparticle catalyst supported by a magnetic nano chain capable of rotation and a preparation method thereof. Background technique [0002] Noble metal palladium nanoparticle catalysts are good catalysts in organic reactions. By using nanoscale noble metal nanoparticles, the contact area with the reactants can be increased, the catalytic reaction can be accelerated, and the catalytic efficiency can be improved. However, when metal nanoparticles are used as catalysts, there are For problems such as easy agglomeration, difficulty in separating the catalyst after the reaction, and low recycling rate, see the literature: [1] Liu Shuang, Li Yong, Shen Wenjie. The influence of crystal phase regulation on the catalytic performance of metal nanoparticles (English) [J]. Catalysis Journal of the Chinese Academy of Sciences, 2015, (09): 1409-141...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J35/10B01J37/34B01J37/08B01J37/03B82Y30/00B82Y40/00C07C1/32C07C15/14
CPCB01J23/8906B01J35/0033B01J35/1019B01J35/1038B01J35/1061B01J37/343B01J35/008B01J37/0018B01J37/036B82Y30/00B82Y40/00C07C1/321C07C15/14
Inventor 陈景露张秋禹
Owner NORTHWESTERN POLYTECHNICAL UNIV
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