Preparation method of palladium-based polyaniline coated carbon nanotube nano catalyst and application of nano catalyst in Heck reaction

A nano-catalyst, carbon nanotube technology, applied in catalytic reactions, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of easy loss, high cost, polluted products, etc., to suppress loss and agglomeration, and effectively recover. effect of separation and cost reduction

Inactive Publication Date: 2018-05-29
GUANGDONG MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a stable and reusable palladium-based polyaniline-wrapped carbon nanotube nanocatalyst and ...

Method used

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  • Preparation method of palladium-based polyaniline coated carbon nanotube nano catalyst and application of nano catalyst in Heck reaction
  • Preparation method of palladium-based polyaniline coated carbon nanotube nano catalyst and application of nano catalyst in Heck reaction
  • Preparation method of palladium-based polyaniline coated carbon nanotube nano catalyst and application of nano catalyst in Heck reaction

Examples

Experimental program
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Embodiment 1

[0031] Preparation of Pd / PANI@CNT

[0032] (1) Purification of carbon nanotubes (CNTs)

[0033] Commercially purchased carbon nanotubes were placed in concentrated nitric acid solution with a mass fraction of 68%, and oxidized and refluxed at 140° C. for 14 hours. The reacted carbon nanotube suspension was first filtered by suction, then repeatedly washed and filtered with deionized water until the pH value of the filtrate was close to neutral, and a large amount of concentrated nitric acid was removed, and then placed in a water bath at 60°C. Stir in a water bath and evaporate to dryness, and finally dry the evaporated black powder in a vacuum oven at 60°C for 24 hours. Store for later use.

[0034] (2) Preparation of Polyaniline (PANI) Wrapped Carbon Nanotubes (PANI@CNT) (PANI@CNT)

[0035] In this paper, the aniline monomer is wrapped on the carbon nanotube by chemical in-situ polymerization. First, 0.25 g of aniline monomer is dissolved in 50 ml of 1 mol / L hydrochloric...

Embodiment 2

[0039] Preparation of Pd / PANI@CNT-1

[0040](1) Purification of carbon nanotubes (CNTs), this part is the same as part (1) in Example 1, and will not be repeated here;

[0041] (2) Preparation of Polyaniline (PANI) Wrapped Carbon Nanotubes (PANI@CNT) (PANI@CNT-1)

[0042] First, 1 g of aniline monomer was dissolved in 50 ml of 1 mol / L hydrochloric acid solution. At the same time, 0.5 g of acid-treated carbon nanotubes were added to another 50 ml of 1 mol / L hydrochloric acid solution, and ultrasonically dispersed for 20 min under ice-bath conditions. Then the hydrochloric acid solution in which the aniline monomer was dissolved and the hydrochloric acid solution in which the carbon nanotubes were dispersed were mixed, and stirred for 20 min. The above carbon tube-aniline mixture was transferred to an ice bath at 0-5 °C, and then ammonium persulfate (0.817 g) was added dropwise to the carbon tube-aniline mixture in 50 ml of 1 mol / L hydrochloric acid solution. The polymerizati...

Embodiment 3

[0046] Preparation of Pd / PANI@CNT-2

[0047] (1) Purification of carbon nanotubes (CNTs), this part is the same as part (1) in Example 1, and will not be repeated here;

[0048] (2) Preparation of Polyaniline (PANI) Wrapped Carbon Nanotubes (PANI@CNT) (PANI@CNT-2)

[0049] First, 2 g of aniline monomer was dissolved in 50 ml of 1 mol / L hydrochloric acid solution. At the same time, 0.5 g of acid-treated carbon nanotubes were added to another 50 ml of 1 mol / L hydrochloric acid solution, and ultrasonically dispersed for 20 min under ice-bath conditions. Then the hydrochloric acid solution in which the aniline monomer was dissolved and the hydrochloric acid solution in which the carbon nanotubes were dispersed were mixed, and stirred for 20 min. Transfer the above carbon tube-aniline mixture to an ice bath at 0-5°C, then dissolve ammonium persulfate (3.268g) in 50ml of 1mol / L hydrochloric acid solution, and add the carbon tube-aniline mixture dropwise . The polymerization reac...

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Abstract

The invention discloses a preparation method of a palladium-based polyaniline coated carbon nanotube nano catalyst, wherein the preparation method mainly includes the following steps: purification ofa carbon nanotube (CNT); preparation of a polyaniline (PANI) coated carbon nanotube (PANI@CNT); and preparation of the Pd/PANI@CNT catalyst. The polyaniline coated carbon nanotube is used, and Pd nanoparticles are loaded on the surface of the PANI@CNT; the formed nano catalyst Pd/PANI@CNT has a quite good reuse performance in a Heck reaction; after reaction is carried out for 10 times, the activity is not reduced. In the prepared Pd/PANI@CNT, a large number of nitrogen-containing functional groups form coordination bonds with Pd, the bonds are quite stable and effectively inhibit the loss andagglomeration of Pd nanoparticles, and thus the cost of the catalyst is effectively reduced. In addition, the catalyst can be effectively recovered and separated, and the contamination and repurification process of the product is prevented.

Description

technical field [0001] The invention relates to the technical field of Heck reaction catalyst synthesis, in particular to a preparation method of a palladium-based polyaniline-wrapped carbon nanotube nanocatalyst and its application in Heck reaction. Background technique [0002] Heck reaction is a kind of carbon-carbon coupling reaction, which is a kind of carbon-carbon coupling reaction between halogenated aromatic compounds and organic compounds with double bonds at the end. In the chemical process, the Heck reaction is usually used to extend the carbon chain. At present, the Heck reaction has been applied in many types of organic synthesis fields, such as: drug synthesis, perfume synthesis, etc. For the Heck reaction, Pd catalyst is the most active catalyst. Traditional Pd-based catalysts are homogeneous Pd catalysts. However, this type of catalyst has serious disadvantages, that is, it is difficult to recover from the product after the reaction, resulting in contamin...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C2/88C07C15/52B82Y30/00
CPCB01J31/06B01J2231/4261B82Y30/00C07C2/88C07C15/52
Inventor 孙文晶余睿江成发冉茂飞赵江浩
Owner GUANGDONG MEDICAL UNIV
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