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Preparation method of magnetic nano palladium catalyst

A technology of magnetic nano and palladium catalysts, which is applied in the preparation of organic compounds, preparation of amino compounds, chemical instruments and methods, etc., to achieve the effects of short time consumption, enhanced binding force, and easy industrial production

Active Publication Date: 2017-06-27
杭州凯大催化金属材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of magnetic nano-palladium catalysts by directly supporting metal palladium on the surface of magnetic nano-iron oxide particles has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: 100 mg Fe 3 o 4 Nanoparticles (purchased from Beijing Deke Daojin Technology Co., Ltd., with an average particle size of 20 nm) were dispersed in 10 mL of 0.1 mol / L tetramethylammonium hydroxide aqueous solution and stirred at room temperature for 1 hour; then 1 mL of saturated NaCl aqueous solution was added to it, After stirring for 5 minutes, the Fe 3 o 4 Aspirate by nanometer, wash three times with deionized water and store in 10 mL DMF.

Embodiment 2

[0016] Embodiment 2: 100 mg Fe 2 o 3 Nanoparticles (purchased from Sigma-Aldrich, with an average particle size of 30 nm) were dispersed in 10 mL of 0.1 mol / L tetramethylammonium hydroxide aqueous solution and stirred at room temperature for 1 hour; then 1 mL of saturated NaCl aqueous solution was added thereto and stirred for 5 minutes Fe 3 o 4 Aspirated by nanometer, washed three times with deionized water and stored in 10 mL DMF.

Embodiment 3

[0017] Embodiment 3: get 5 mL embodiment 1 gained Fe 3 o 4 DMF dispersion of nanoparticles, to which 5 mLDMF, 10 mL ethylene glycol and 10 mg PdCl were added sequentially 2 , and sonicated for 1 hour; the nanoparticles were sucked out with a magnet, and washed 3 times with deionized water to obtain the magnetic nano-palladium catalyst nano-Fe 3 o 4 -Pd, keep it in 5 mL methanol. The palladium content in this magnetic nano-palladium catalyst was determined to be 5.2% by ICP-OES.

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Abstract

The invention discloses a preparation method of a magnetic nano palladium catalyst, wherein the preparation method comprises the steps: firstly, treating iron oxide nanoparticles with a tetramethylammonium hydroxide aqueous solution; secondly, carrying out ultrasonic treatment on the iron oxide nanoparticles and a metal palladium salt in a mixed solvent composed of alcohol and N,N-dimethyl formamide; and finally, absorbing the magnetic nano palladium catalyst out from the mixed solvent with a magnet, respectively washing with deionized water and methanol, and then preserving in methanol. The preparation method is simple and easy to implement; the prepared magnetic nano palladium catalyst has high activity, can be used in catalysis of nitro hydrogenation reduction reaction, and moreover, is easily absorbed out from the reaction mixture with the magnet and is repeatedly used.

Description

technical field [0001] The invention relates to a method for preparing a magnetic nano-palladium catalyst, in particular to a method for preparing a magnetic nano-palladium catalyst by directly supporting metal palladium nanoparticles on the surface of magnetic nano-iron oxide particles. Background technique [0002] Palladium / carbon and various other supported palladium catalysts have been widely used in modern organic synthesis to efficiently catalyze a variety of organic chemical reactions, such as the catalytic hydrogenation of alkenes or nitro compounds. These palladium catalysts have excellent catalytic performance, but their separation requires filtration operations, making it difficult to achieve continuous reaction production in the same reactor. [0003] Magnetic nano-iron oxide particles are a kind of inorganic nanomaterials developed in recent years. Due to their unique superparamagnetic properties in the liquid phase dispersion state, they have attracted extensi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07C209/36C07C211/46
CPCY02P20/582
Inventor 端木传嵩赵峰钱国庆黄秀蓉周浩杰许兴友孙永明
Owner 杭州凯大催化金属材料股份有限公司