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Palladium composite catalyst and its preparation method and application

A composite catalyst and catalyst technology, applied in the direction of catalytic reaction, preparation of amino compounds, chemical instruments and methods, etc., can solve the problems of reducing the quality of aromatic amine products, etc.

Active Publication Date: 2021-09-07
JIANGSU SINOCOMPOUND CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet the aromatic amine product that the preparation method of present aromatic amine makes not only has the residue of cyclopalladium catalyst, also contains the residue of the alkali metal in these strong bases; Therefore greatly reduces the quality of aromatic amine product

Method used

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  • Palladium composite catalyst and its preparation method and application

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preparation example Construction

[0041] Another embodiment of the present invention provides a kind of preparation method of palladium composite catalyst, comprises the steps:

[0042] Raw materials are provided according to the content ratio of the cyclopalladium catalyst and the solid base in the palladium composite catalyst of any one of the above;

[0043] The cyclopalladium catalyst and the solid base are mixed in a solvent, and the solvent is evaporated to obtain a palladium composite catalyst.

[0044] It can be understood that the raw materials used in the above preparation method are provided according to the content ratio of the cyclopalladium catalyst and the solid base in the palladium composite catalyst.

[0045] The above preparation method mixes the cyclopalladium catalyst and the solid base in a solvent, wherein the cyclopalladium catalyst is dissolved in the solvent as a homogeneous catalyst, and with the evaporation of the solvent, the homogeneous catalyst is precipitated on the surface of the...

Embodiment 1

[0071] (1) Preparation of palladium composite catalyst:

[0072] 1 gram of cyclopalladium catalyst was dissolved in 100 grams of dichloromethane, 199 grams of 15% magnesium oxide modified alumina was added and stirred for 4 hours, and the dichloromethane was evaporated to dryness at 40 degrees Celsius to obtain 200 grams of palladium composite catalyst.

[0073] (2) Catalytic reaction of palladium composite catalyst:

[0074] Add 1 gram of the palladium composite catalyst prepared above, 0.05mol of X-phos, 0.5mol of aniline and 0.5mol of chlorobenzene, dissolve in 10L of dioxane, heat up to 100°C, and react for 10 minutes; add Methanol is heated to 60 degrees Celsius, the cyclopalladium catalyst is reduced on the surface of the solid base, the solid and liquid are separated, the solid is recovered, and the diphenylamine product is obtained from the filtrate, and the reaction yield is 99%. Use HPLC to detect the diphenylamine product, and the product purity is 98%.

Embodiment 2

[0076] (1) Preparation of palladium composite catalyst:

[0077] Dissolve 1 gram of cyclopalladium catalyst in 100 grams of dichloromethane, add 199 grams of 25% magnesia-modified silicon oxide and stir for 4 hours, and evaporate the dichloromethane to dryness at 40 degrees Celsius to obtain 200 grams of palladium composite catalyst.

[0078] (2) Catalytic reaction of palladium composite catalyst:

[0079] Add 1 gram of the palladium composite catalyst prepared above, 0.05mol of X-phos, 0.5mol of aniline and 0.5mol of chlorobenzene, dissolve in 10L of dioxane, heat up to 100°C, and react for 10 minutes; add Methanol is heated to 60 degrees Celsius, the cyclopalladium catalyst is reduced on the surface of the solid base, the solid and liquid are separated, the solid is recovered, and the diphenylamine product is obtained from the filtrate, and the reaction yield is 99%. Use HPLC to detect the diphenylamine product, and the product purity is 98%.

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Abstract

The invention relates to a palladium composite catalyst and its preparation method and application, wherein the palladium composite catalyst comprises a cyclopalladium catalyst and a solid base, and the cyclopalladium catalyst is dispersed on the surface of the solid base; the solid base is oxidized Magnesium-modified metal oxide; the mass content of the total amount of the cyclopalladium catalyst in the total mass of the cyclopalladium catalyst and the solid base is 0.1% ~ 10%, and the magnesium oxide is in the magnesium oxide and the The mass content of the two metal oxides in the total mass is 10%-30%. In the present invention, the metal oxide modified by magnesia replaces the strong base by selecting a specific type of solid base, providing the solid-supported base required for the reaction, and simultaneously dispersing the cyclopalladium catalyst on the surface of the solid base. When the palladium composite catalyst is used for the catalysis of the carbon-nitrogen coupling reaction, the problem of alkali metal residues caused by the use of a strong base is avoided, and the catalytic efficiency of the carbon-nitrogen coupling reaction is effectively improved on the basis of lower metal residues.

Description

technical field [0001] The invention relates to the technical field of chemical catalysis, in particular to a palladium composite catalyst and its preparation method and application. Background technique [0002] The Buchwald-Hartwig carbon-nitrogen coupling reaction is a cross-coupling reaction of aryl halides and organic amines in the presence of a palladium catalyst and a base, and is an important method for the synthesis of arylamine compounds. The Buchwald–Hartwig type of reaction was first discovered in 1986 by Lev M. Yagupolskii in Ukraine. Afterwards, the Buchwald and Hartwig teams in the United States rediscovered this reaction in 1994, respectively. Wherein, the organic amine can be a primary amine or a secondary amine, and the substituent on the organic amine can be any organic group. [0003] The traditional Buchwald–Hartwig carbon-nitrogen coupling reaction is carried out under strong base, and the strong base generally used is potassium carbonate, cesium carb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/24C07C209/10C07C211/55
CPCB01J31/2414B01J2231/4283B01J2531/824C07C209/10C07C211/55
Inventor 钱棋春倪自林王正
Owner JIANGSU SINOCOMPOUND CATALYST
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