Method for activating carbon nanotube-supported palladium nanoparticle catalyst and application thereof

A technology of carbon nanotubes and palladium nanometers, which is applied in the field of new green and environmentally friendly activated carbon nanotube-loaded palladium nanoparticle catalysts, can solve the problems of insufficient proven reserves, waste, and low utilization rate, so as to reduce energy consumption and improve catalytic performance , the effect of simple application equipment

Active Publication Date: 2019-07-02
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Precious metals have important applications in the fields of industrial catalysis, aviation manufacturing, and nanomaterial synthesis. Although our country is one of the countries with richer reserves of precious metals in the world, there are still few extra-large deposits, insufficient proven reserves, low utilization rate, and waste serious problems

Method used

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  • Method for activating carbon nanotube-supported palladium nanoparticle catalyst and application thereof
  • Method for activating carbon nanotube-supported palladium nanoparticle catalyst and application thereof
  • Method for activating carbon nanotube-supported palladium nanoparticle catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of carbon nanotube-supported palladium nanoparticles catalyst

[0025] 1) Take 60mg of ascorbic acid, 105mg of PVP and 600mg of potassium bromide, add 8mL of distilled water to dissolve, stir to dissolve, put it in an oil bath at 80°C for 1 hour, then quickly add 3mL of Na 2 PdCl 4 Aqueous solution (contains Na 2 PdCl 4 57 mg), continued to react in an oil bath at 80°C for 3 h, centrifuged, and dried the product in a vacuum oven to obtain a bright black solid powder, namely palladium nanoparticles.

[0026] 2) Put 2 mL of palladium nanoparticle solution with a concentration of 1 mg / mL in a beaker, add absolute ethanol to dilute to 15 mL, sonicate for three minutes, and pour it into a titration funnel for use.

[0027] 3) Weigh 100mg of carbon nanotubes (LNT) into a 100mL round-bottomed flask, add 20mL of ethanol, and after ultrasonication for 8 minutes, start to drop the ethanol solution of palladium nanoparticles, keep the flow rate for 1-2 seconds ...

Embodiment 2

[0033] (1) Application of Activated Carbon Nanotube-supported Palladium Nanoparticle Catalysts in Suzuki Reaction

[0034] 1. Activation: The carbon nanotube-supported palladium nanoparticle catalyst prepared in Example 1 was placed in a container, and the method was the same as step (2) of Example 1, and treated at 60° C. for 4 hours.

[0035] 2. Mix 0.5853g of phenylboronic acid, 1.1057g of potassium carbonate, 40mL of aqueous ethanol (ethanol:water=5:3v / v), and 10mg of activated carbon nanotube-supported palladium nanoparticle catalyst, and mix them uniformly, and place them in an oil bath at 60°C After stirring for 10 minutes, 0.44 mL of bromobenzene was added to continue the reaction. A small amount of product was taken at 15, 25, 35 and 50 minutes respectively, and the reaction product was analyzed by GC. After 25 minutes of reaction, the conversion rate was 50%.

Embodiment 3

[0039] 1. Activation: The carbon nanotube-loaded palladium nanoparticle catalyst prepared in Example 1 was placed in a container, and the method was the same as step (2) of Example 1, and treated at 80° C. for 4 hours.

[0040]2. Mix 0.5853g of phenylboronic acid, 1.1057g of potassium carbonate, 40mL of aqueous ethanol (ethanol:water=5:3v / v), and 10mg of activated carbon nanotube-supported palladium nanoparticle catalyst, and mix them uniformly, and place them in an oil bath at 60°C After stirring for 10 minutes, 0.44 mL of bromobenzene was added to continue the reaction. A small amount of product was taken at 15, 25, 35 and 50 minutes respectively, and the reaction product was analyzed by GC. After 25 minutes of reaction, the conversion rate was 90%.

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Abstract

The invention discloses a method for activating a carbon nanotube supported palladium nanoparticle catalyst and application thereof, and belongs to the technical field of the improvement of the performance of an inorganic metal nanoparticle catalyst. A carbon nanotube supported palladium nanoparticle catalyst is placed in a vessel and treated with water vapor for 2-10h at 60 to 200 DEG C. The supported palladium catalyst treated with the water vapor is used for Suzuki coupling reaction. The catalyst has the advantages of stable performance, good catalytic activity, green and environment-friendly catalyst activation way, no any by-products, and simple and efficient equipment. The activated supported palladium catalyst can significantly improve the catalytic performance of the Suzuki coupling reaction.

Description

technical field [0001] The invention relates to the technical field of catalyst improvement, in particular to a novel green and environment-friendly method for activating carbon nanotube-loaded palladium nanoparticle catalysts and its application. Background technique [0002] One of the important components of supported catalysts is metal nanoparticles, which are usually composed of hundreds or thousands of atoms. At present, regarding the preparation of metal nanoparticles, the commonly used colloidal method has been proved to be particularly suitable for the generation and shape control of small nanoparticles, and the prepared metal nanoparticles have excellent catalytic properties. However, in order to control the shape and size of nanoparticles, surfactants are usually used in the process of preparing nanoparticles, and the surfactant ligands will be deposited on the surface of metal nanoparticles, which can severely cover the surface atoms of nanoparticles, and then S...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07C1/32C07C15/14
CPCB01J23/44C07C1/321C07C2523/44C07C15/14
Inventor 杨黎妮程广振邢丽娜程春霞夏立新
Owner LIAONING UNIVERSITY
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