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Nano-Pd magnetic catalyst, its preparation method, and its use in liquid phase catalysis reaction

A catalyst and magnetic technology, applied in the field of nano-magnetic catalysts, can solve problems such as complex processes, reduce separation costs and improve reuse efficiency.

Inactive Publication Date: 2014-02-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for nanoscale catalysts, the process of filtration operation is more complicated

Method used

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  • Nano-Pd magnetic catalyst, its preparation method, and its use in liquid phase catalysis reaction

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Effect test

Embodiment 1

[0020] (1) Weigh 13.4g FeCl 3 ·6H 2 O was dissolved in 86.6g of deionized water to make a solution, and 4.1g of sodium acetate was weighed and dissolved in 45.9g of ethylene glycol to make a solution. At the temperature of a water bath at 30°C and under stirring conditions, it was added dropwise to the solution containing N 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0021] (2) Weigh the prepared magnetic Fe 3 o 4 Add 5.8g of granules to 44.2g of ethanol, add dropwise 20g of sodium silicate solution with a mass concentration of 5% and cetyltrimethyl bromide with a mass concentration of 0.2% at the same time at a water bath temperature of 30°C under stirring conditions Ammonium chloride (CTAB) ethanol solution 5g, after t...

Embodiment 2

[0025] (1) Weigh 20.3g FeCl 3 ·6H 2 O was dissolved in 79.7g of deionized water to make a solution, and 6.2g of sodium acetate was weighed and dissolved in 43.8g of ethylene glycol to make a solution. At the temperature of a water bath at 30°C and under stirring conditions, it was added dropwise to the solution containing N 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0026] (2) Weigh the prepared magnetic Fe 3 o 4 Add 6.9g of granules to 43.1g of ethanol, add 20g of sodium silicate solution with a mass concentration of 10% and hexadecyltrimethyl bromide with a mass concentration of 0.2% at the same time under stirring conditions at a water bath temperature of 30°C Ammonium chloride (CTAB) ethanol solution 10g, after the ...

Embodiment 3

[0030] (1) Weigh 27.0g FeCl 3 ·6H 2 O was dissolved in 73.0g deionized water to make a solution, and 8.2g of sodium acetate was weighed and dissolved in 41.8g of ethylene glycol to make a solution, which was added dropwise at the temperature of a water bath at 30°C under stirring conditions 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0031] (2) Weigh the prepared magnetic Fe3 o 4 Add 9.3g of granules to 40.7g of ethanol, add dropwise 15g of sodium silicate solution with a mass concentration of 15% and cetyltrimethyl bromide with a mass concentration of 0.2% at the same time at a water bath temperature of 30°C under stirring conditions Ammonium chloride (CTAB) ethanol solution 15g, after the dropwise addition, ammonia solu...

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Abstract

The invention relates to a nano-Pd magnetic catalyst, its preparation method, and its use in a liquid phase catalysis reaction, and belongs to the technical field of nanometer magnetic catalysts. A super-paramagnetic Fe3O4 core is made, a layer of meso-porous SiO2 is formed on the layer of the magnetic Fe3O4 core by adopting an ultrasonic wave method with cetyltrimethylammonium bromide as a template and sodium silicate as a silicon source, the obtained material is dried, and the material is roasted under the protection of N2 to remove the template in order to prepare a magnetic SiO2@Fe3O4 nanosphere. A Pd catalysis active component is assembled on the meso-porous SiO2 shell on the surface of the magnetic SiO2@Fe3O4 nanosphere by adopting the ultrasonic wave method with the magnetic SiO2@Fe3O4 nanosphere as a core to prepare the magnetic Pd / SiO2@Fe3O4 catalyst. Pd catalysis active component particles are embedded in meso-porous SiO2 to form a highly dispersed nano-Pd catalysis active component, so the activity of the catalyst is improved, and the loss of Pd in the reaction process is avoided.

Description

technical field [0001] The invention relates to a preparation method of a magnetic catalyst for assembling nano Pd catalytic active component particles on the surface of a magnetic core carrier and its use in a liquid phase catalytic reaction, belonging to the technical field of nano magnetic catalysts. Background technique [0002] Under the action of a catalyst, bromobenzene and butyl acrylate can form C-C coupled organic compounds, which are widely used in the synthesis of dyes, medicines, pesticides, and fine chemicals. Most of the traditional catalysts for this type of C-C coupling reaction are homogeneous catalysts with the noble metal Pd as the main active component. However, due to the difficulty in separation and recovery of homogeneous catalysts, the Pd catalytically active components are loaded on various commonly used catalyst supports. On the other hand, the prepared supported Pd-based catalyst can realize the separation of the catalyst and the reactant by filte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J35/02C07C69/618C07C67/343B01J35/00
Inventor 季生福刘雪菲杨浩张丹妮
Owner BEIJING UNIV OF CHEM TECH
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