Preparation method of magnetic nanoparticle supported precious metal catalyst

A technology of magnetic nanoparticles and noble metal catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc. Increase and other problems, to achieve high specific surface area, fast recycling, fast separation effect

Active Publication Date: 2017-02-22
INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, whether it is an organic polymer carrier or an inorganic carrier, its catalytic activity, stability and recycling performance need to be further improved, and its application range is quite limited.
In recent years, magnetic nanoparticles have received widespread attention as catalyst supports, and the technical means is to use magnetic Fe 3 o 4 The surface of nanoparticles is coated with a thin layer of silica gel, and various organic ligands are connected to the hydroxyl groups on the surface, but the content of precious metals is also low, resulting in an increase in usage, and the activity of the nanoparticles is gradually reduced due to the weak ligands during recycling.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation method of magnetic nanoparticle supported palladium catalyst is as follows:

[0019] ①Add 2g of nanometer iron ferric oxide and 30g of toluene into a 250ml four-necked flask equipped with a thermometer, agitator, and condenser tube. After ultrasonically dispersing for 2 hours, add 5g of deionized water, 6g of absolute ethanol, and 60g of γ -Mercaptopropyltriethoxysilane, using acetic acid to adjust the pH of the system to 5, stirring at 60°C for 8h, the product was filtered, washed, and dried to obtain magnetic nanoparticles with mercapto groups on the surface;

[0020] ②Add 5g of magnetic nanoparticles with mercapto groups on the surface and 30g of toluene prepared in step ① into a 250ml four-neck flask for ultrasonic dispersion for 2h, then add 20g of diphenyl-p-styrylphosphine and 0.02g of photoinitiator benzophenone, React for 10 hours under ultraviolet light irradiation. After the reaction, the suspension is separated by magnet, washed and dried to ...

Embodiment 2

[0023] The preparation method of magnetic nanoparticle supported platinum catalyst is as follows:

[0024] ①In a 250ml four-necked flask equipped with a thermometer, agitator, and a condenser, add 4g of nano-ferric oxide and 50g of xylene, and after ultrasonic dispersion for 4 hours, add 8g of deionized water, 10g of absolute ethanol, and 100g of γ-Mercaptopropyltrimethoxysilane, using acetic acid to adjust the pH of the system to 7, stirring at 80°C for 6 hours, the product was filtered, washed, and dried to obtain magnetic nanoparticles with mercapto groups on the surface;

[0025] ②Add 3g of magnetic nanoparticles with mercapto groups on the surface and 10g of xylene prepared in step ① into a 250ml four-neck flask for ultrasonic dispersion for 1h, then add 100g of 4-dimethylaminostyrene and 0.05g of photoinitiator 1-hydroxy Cyclohexyl phenyl ketone was reacted for 6 hours under ultraviolet light irradiation. After the reaction, the suspension was separated by magnet, washed...

Embodiment 3

[0028] The preparation method of magnetic nanoparticle supported gold catalyst is as follows:

[0029] ①Add 3g of nanometer iron ferric oxide and 40g of toluene into a 250ml four-neck flask equipped with a thermometer, agitator, and condenser tube. After ultrasonic dispersion for 2 hours, add 6g of deionized water, 8g of absolute ethanol, and 60g of γ -Mercaptopropyltrimethoxysilane, using acetic acid to adjust the pH of the system to 6, stirring at 70°C for 8h, the product was filtered, washed, and dried to obtain magnetic nanoparticles with mercapto groups on the surface;

[0030] ②Add 5g of magnetic nanoparticles with mercapto groups on the surface prepared in step ① and 30g of isopropanol into a 250ml four-neck flask for ultrasonic dispersion for 2h, then add 80g of vinyl diphenylphosphine and 0.04g of photoinitiator 2-hydroxy-2 -Methyl-1-phenyl-1-acetone, reacted for 8 hours under ultraviolet light irradiation, after the reaction, the suspension was separated by magnet, w...

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PUM

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Abstract

The preparation method of a magnetic nanoparticle supported precious metal catalyst comprises the following steps: grafting the silane coupling agent containing thiol to the surface of magnetic ferriferrous oxide nanoparticles, using the thiols on the surface to conduct the click reaction with vinyl organic ligand compound to form magnetic nanoparticle supporting complex, complexing with precious metal salt to acquire the magnetic nanoparticle supported precious metal catalyst. According to the method, the click chemical reaction is used to combine the magnetic nanoparticle surface and the vinyl organic ligand compound by covalent bonds, and solidly bind the ligand to the magnetic nanoparticle. At the same time the method can guarantee that the ligand is far from the supporter, and can coordinate with the precious metal in a better way to achieve the effect of homogeneous catalysis. Moreover under the external magnetic field, the catalyst is easy to be magnetized, and has the advantage of fast separation, fast recycling and reusable features. The method can lower the production cost, and enhance the production efficiency. The catalyst prepared by the method can be used in the coupling reaction and addition reaction of metal catalytic reaction.

Description

technical field [0001] The invention relates to a method for preparing a magnetic nanoparticle-loaded noble metal catalyst based on a click chemistry method, which belongs to the technical field of catalysts. Background technique [0002] Noble metal catalyzed reaction is one of the important means of organic chemical synthesis methods, but these noble metal catalysts are difficult to sort and recover from the reaction system, which increases the cost of the reaction, and even organometallic catalysis such as palladium metal will cause palladium black during the reaction process, which not only reduces the activity of the catalyst , but also pollute the reaction product, which is greatly limited in practical application. Therefore, more and more scientific researchers are solving these problems through the research on supported catalysts, striving to maintain the high efficiency of homogeneous catalysts, solve the recycling of catalysts, and achieve the goals of minimum cons...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J35/10
CPCB01J31/28B01J35/0033B01J35/1004B01J2531/18B01J2531/822B01J2531/824B01J2531/828
Inventor 游胜勇饶国华蔡明中陈衍华董晓娜李玲谌开红徐彩凤易飞燕
Owner INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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