Palladium-based dopamine-coated magnetic carbon nano-tube catalyst, and preparation method and application thereof

A technology of magnetic carbon nanotubes and palladium-based dopamine, which is applied in the direction of catalyst activation/preparation, carbon compound catalysts, catalysts, etc., can solve the problems of Pd filtration and loss in the active center, and cannot be applied in the field of pharmaceutical synthesis, so as to suppress the loss, The effect of excellent magnetic separation performance without performance degradation

Inactive Publication Date: 2017-10-17
GUANGDONG MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current magnetic catalysts still have the problem of leaching and loss of the active center Pd in ​​the reaction, making it impossible to apply in the field of pharmaceutical synthesis

Method used

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  • Palladium-based dopamine-coated magnetic carbon nano-tube catalyst, and preparation method and application thereof

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preparation example Construction

[0024] A method for preparing a palladium-based dopamine-wrapped magnetic carbon nanotube catalyst proposed in an embodiment of the present invention, comprising:

[0025] 1) Place the carbon nanotubes in a mass fraction of 68% concentrated sulfuric acid, reflux oxidation at 130-150° C. for 10-15 hours, to remove transition metal catalysts and amorphous carbon in the production process of carbon nanotubes, and Carboxyl and other functional groups are grafted on the surface; after the reaction is completed, the mixed solution is cooled, the solid is filtered out, and washed with ethanol and deionized water several times in sequence; the solid mixture is placed in a 60°C water bath and continuously stirred to prevent carbon nanotubes from agglomerating ; After the solid was slowly evaporated to dryness, the black powder sample was placed in a vacuum oven at 60°C for 24 hours to obtain carboxylated carbon nanotubes (CNT);

[0026] 2) Dissolving the nickel salt in a mixed solution...

Embodiment 1

[0037] A method for preparing a palladium-based dopamine-wrapped magnetic carbon nanotube catalyst proposed in an embodiment of the present invention, comprising:

[0038] 1) Place 1g of carbon nanotubes in mass fraction in 68% concentrated sulfuric acid (25mL), reflux oxidation at 140°C for 14h to remove transition metal catalysts and amorphous carbon in the production process of carbon nanotubes, and Carboxyl and other functional groups are grafted on the surface; after the reaction is completed, the mixed solution is cooled, the solid is filtered out, and washed with ethanol and deionized water several times in sequence; the solid mixture is placed in a 60°C water bath and continuously stirred to prevent carbon nanotubes from agglomerating ; After the solid was slowly evaporated to dryness, the black powder sample was placed in a vacuum oven at 60°C for 24 hours to obtain carboxylated carbon nanotubes (CNT);

[0039]2) Dissolving nickel nitrate in a mixed solution of ethano...

Embodiment 2

[0044] A method for preparing a palladium-based dopamine-wrapped magnetic carbon nanotube catalyst proposed in an embodiment of the present invention, comprising:

[0045] 1) Place 1g of carbon nanotubes in mass fraction in 68% concentrated sulfuric acid (25mL), reflux oxidation at 130°C for 15h to remove transition metal catalysts and amorphous carbon in the production process of carbon nanotubes, and Carboxyl and other functional groups are grafted on the surface; after the reaction is completed, the mixed solution is cooled, the solid is filtered out, and washed with ethanol and deionized water several times in sequence; the solid mixture is placed in a 60°C water bath and continuously stirred to prevent carbon nanotubes from agglomerating ; After the solid was slowly evaporated to dryness, the black powder sample was placed in a vacuum oven at 60°C for 24 hours to obtain carboxylated carbon nanotubes (CNT);

[0046] 2) dissolving nickel nitrate in a mixed solution of ethan...

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Abstract

The invention relates to a palladium-based dopamine-coated magnetic carbon nano-tube catalyst and application thereof. A preparation method comprises the following steps: (1) oxidizing carbon nano-tubes to obtain carboxylic carbon nano-tubes; (2) dissolving a nickel salt in a mixed solution of ethyl alcohol and water, adding the carboxylic carbon nano-tubes, performing ultrasonic treatment, drying and roasting to obtain nickel-filled carboxylic carbon nano-tubes; (3) dispersing the nickel-filled carboxylic carbon nano-tubes in Tris buffering liquid, adding dopamine, stirring, and performing centrifugal drying to obtain poly-dopamine-coated magnetic carbon nano-tubes; and (4) dispersing the poly-dopamine-coated magnetic carbon nano-tubes in an aqueous solution of a palladium salt, performing ultrasonic treatment, heating, stirring, evaporating, drying, and reducing to obtain the palladium-based dopamine-coated magnetic carbon nano-tube catalyst. The palladium-based dopamine-coated magnetic carbon nano-tube catalyst has excellent magnetic separating performance and can be effectively separated from a liquid phase after the completion of a reaction; and the recycling rate of the catalyst is effectively improved.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a palladium-based dopamine-wrapped magnetic carbon nanotube catalyst and its application. Background technique [0002] The Heck reaction is one of the main reactions for the formation of C-C bonds. It plays a very important role in the synthesis of important compounds such as drugs, dyes, and essences. So far, Pd is the main catalyst for the Heck reaction. Traditional catalysts used in industry often have many disadvantages. For example, homogeneous catalysts are difficult to separate from the solution during the reaction, resulting in product pollution, which in turn increases the steps of product purification, making the reaction cost high and the process complicated; Noble metal catalysts are expensive, resulting in very high reaction costs; some Pd catalysts containing phosphine ligands have very high activity and selectivity. But such catalysts are very polluting to the environm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J37/08B01J37/18C07C15/52C07C2/86
CPCB01J23/892B01J35/0013B01J35/0033B01J35/006B01J35/008B01J37/088B01J37/18C07C2/861C07C2523/89C07C15/52Y02P20/584
Inventor 孙文晶余睿江成发冉茂飞赵江浩
Owner GUANGDONG MEDICAL UNIV
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