Multilevel core-shell structure magnetic nano gold catalyst and preparation method thereof

A magnetic nanometer, core-shell structure technology, applied in the preparation of carbon-based compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of complex preparation methods of magnetic nanocomposites, and achieve Effects of excellent catalytic activity and selectivity for alcohol oxidation and strong superparamagnetic properties

Inactive Publication Date: 2012-06-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation method of the

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of magnetic substances

[0021] Weigh 3.25g (0.012mol) ferric chloride hexahydrate (FeCl 3 ·6H 2 O) and 8.64g (0.063mol) sodium acetate trihydrate (CH 3 COONa·3H 2 O) dissolved in 80ml of ethylene glycol, transferred to a 100ml reaction kettle, crystallized at 200°C for 8 hours, naturally cooled to room temperature, magnetically separated by NdFeB permanent magnets, washed 3 times with ethanol and deionized water, respectively, During the washing process, NdFeB permanent magnets are still used for magnetic separation, and dried at 60 ° C for 24 hours to obtain a black powder, which is recorded as Fe 3 o 4 .

[0022] (2) Preparation of core-shell magnetic carrier

[0023] Weigh 1.0g Fe 3 o 4 The solid was dispersed in 100ml methanol aqueous solution (V 甲醇 :V 水 =1), ultrasonically dispersed for 5 minutes, then transferred to a round-bottomed flask, and stirred at room temperature.

[0024] Prepare NaOH(0.10mol / L) / Na 2 CO 3 (0.05mol / L) mixed al...

Embodiment 2

[0030] (1) Preparation of magnetic substances

[0031] Weigh 3.25g (0.012mol) ferric chloride hexahydrate (FeCl 3 ·6H 2 O) and 8.64g (0.063mol) sodium acetate trihydrate (CH 3 COONa·3H 2 O) dissolved in 80ml of ethylene glycol, transferred to a 100ml reaction kettle, crystallized at 200°C for 8 hours, naturally cooled to room temperature, magnetically separated by NdFeB permanent magnets, washed 4 times with ethanol and deionized water, respectively, During the washing process, NdFeB permanent magnets are still used for magnetic separation, and dried at 80 ° C for 18 hours to obtain a black powder, which is recorded as Fe 3 o 4 .

[0032] (2) Preparation of core-shell magnetic carrier

[0033] Weigh 2.0g Fe 3 o 4 The solid was dispersed in 80ml methanol aqueous solution (V 甲醇 :V 水 =0), ultrasonically dispersed for 10 minutes, then transferred to a round-bottomed flask, and stirred at room temperature.

[0034] Prepare NaOH(0.20mol / L) / Na 2 CO 3 (0.10mol / L) mixed al...

Embodiment 3

[0040] (1) Preparation of magnetic substances

[0041] Weigh 3.25g (0.012mol) ferric chloride hexahydrate (FeCl 3 ·6H 2 O) and 8.64g (0.063mol) sodium acetate trihydrate (CH 3 COONa·3H 2 O) dissolved in 80ml of ethylene glycol, transferred to a 100ml reaction kettle, crystallized at 200°C for 8 hours, naturally cooled to room temperature, magnetically separated by NdFeB permanent magnets, washed 5 times with ethanol and deionized water respectively, During the washing process, NdFeB permanent magnets are still used for magnetic separation, and dried at 100 ° C for 12 hours to obtain a black powder, which is recorded as Fe 3 o 4 .

[0042] (2) Preparation of core-shell magnetic carrier

[0043] Weigh 3.0g Fe 3 o 4 The solid was dispersed in 100ml methanol aqueous solution (V 甲醇 :V 水 =0.5), ultrasonically dispersed for 15 minutes, then transferred to a round-bottomed flask, and stirred at room temperature.

[0044] Prepare NaOH(0.15mol / L) / Na 2 CO 3 (0.10mol / L) mixed...

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Abstract

The invention relates to a multilevel core-shell structure magnetic nano gold catalyst and a preparation method thereof, belonging to the field of magnetic nano catalytic material. A core-shell structure composite which is formed by taking a lamellar double-hydroxyl composite metal oxide (M2+)(M3+)-LDHs as a shell and Fe3O4 magnetic nano particles as a core is taken as a carrier to load nano goldparticles, the shell (M2+)(M3+)-LDHs nano slice is vertically intersected and epitaxially grow and has a honeycomb appearance, the gold nano particles are carried and loaded on the surface of the (M2+)(M3+)-LDHs nano slice, and H2 is reduced, thus the multilevel core-shell structure magnetic nano gold catalyst Fe3O4@(M2+)(M3+)-LDHs@Au is obtained. The invention has the advantages that the multilevel core-shell structure magnetic nano gold catalyst has stronger superparamagnetism and also has excellent catalytic alcohol oxidation activity and selectivity, 1-phenethyl alcohol oxidation is takenas a probe reaction, the air is taken as an oxidant for reaction at the temperature of 80 DEG C, reaction is carried out for 3 hours, and yield of phenylacetaldehyde is 99%; meanwhile, the preparation method is simple, the catalyst is conveniently enriched and recycled by adding an external magnetic field after reaction is finished, and catalytic activity of the catalyst is not reduced after the catalyst is reused for five times.

Description

technical field [0001] The invention belongs to the technical field of magnetic nano-catalysis materials, and in particular provides a magnetic nano-gold catalyst with a multi-level core-shell structure and a preparation method thereof. technical background [0002] Oxidation reactions are an important process in organic synthesis and play an important role in the functionalization of reaction intermediates for pharmaceuticals, fine chemicals, and agricultural chemicals. Whether it is laboratory preparation or industrial production, the oxidation process of alcohols into carbonyl compounds plays an important role in various types of oxidation transformations. In terms of chemical properties and various uses, carbonyl compounds occupy a special important position, and they are often the starting materials for synthesis. Aldehyde and ketone compounds have various structures and are widely used. The annual production of carbonyl compounds in the world exceeds one million tons,...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J35/10C07C47/52C07C45/38B82Y25/00B82Y30/00
Inventor 张慧米飞刘婷马跃文殷双涛袁方龙
Owner BEIJING UNIV OF CHEM TECH
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