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A kind of preparation method, catalyst and application of catalyst obtained by modifying palladium

A catalyst and compound technology, applied in the field of catalyst preparation, can solve the problems of increasing the use of precious metals, complicated preparation methods, difficult industrial-scale application and production, etc., and achieves a simple and fast preparation method, good stability, and good stability.

Active Publication Date: 2021-12-03
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high activity of palladium, the traditional method often needs to poison some sites to have good selectivity to alkynes, which leads to very low activity of the catalyst, increases the use of noble metals, and increases the cost; another On the one hand, the method for the preparation of selective semi-hydrogenation catalysts is relatively complicated, especially for catalysts that only have selective semi-hydrogenation of intermediate alkynes, and it is difficult to carry out industrial-scale application production

Method used

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  • A kind of preparation method, catalyst and application of catalyst obtained by modifying palladium
  • A kind of preparation method, catalyst and application of catalyst obtained by modifying palladium
  • A kind of preparation method, catalyst and application of catalyst obtained by modifying palladium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1: Catalyst prepared by two-dimensional palladium nanosheets for semi-hydrogenation reaction

[0052] S1: Disperse two-dimensional palladium nanosheets (Pd Ns) in a DMF solvent, and react with a hydrogen gas of one atmospheric pressure for 10 minutes, maintain the gas atmosphere, and add 3,4-difluorothiophenol as a ligand M, so that M: The molar ratio of Pd is 0.3:1, the stirring time is 30min, the stirring temperature is 80°C, and M-Pd is prepared after suction filtration and drying for 12h 4 The S Ns catalyst is ready for use (M is 3,4-difluorothiophenol).

[0053] S2: The prepared M-Pd 4 S Ns catalyst for semi-hydrogenation reaction with 1-phenyl-1-propyne as the substrate, the reaction steps are: transfer 20ml of ethanol to a 48ml reaction flask, take 2mmol of the substrate into the reaction flask and sonicate Disperse for 1 min, set the temperature at 60°C, add a corresponding amount of catalyst, the molar ratio of substrate to Pd is 2000:1, replace hydro...

Embodiment 2

[0054] Embodiment 2: the stability that catalyst of the present invention applies mechanically

[0055] S1: Disperse Pd / C with a Pd mass fraction of 5% in a DMF solvent, pass a hydrogen atmosphere of hydrogen to react for 10 minutes, keep the gas atmosphere, add 3,4-difluorothiophenol as ligand M, so that M The molar ratio of :Pd is 0.4:1, the stirring time is 60min, the stirring temperature is 80°C, and the M-Pd is prepared after suction filtration and drying for 12h 4 The S / C catalyst is ready for use (M is 3,4-difluorothiophenol). figure 2 For the preparation of M-Pd 4 The XRD figure of S / C catalyst, it can be seen that Pd is formed in the catalyst preparation process of the present invention 4 S phase.

[0056] S2: Pd / C with the same molar mass of Pd and the prepared M-Pd 4 The S / C catalysts respectively carry out semi-hydrogenation reaction with 1-phenyl-1-propyne as the substrate. The reaction steps are: transfer 20ml of ethanol to a 48ml reaction flask, and take 2m...

Embodiment 3

[0059] S1: Disperse Pd / X with the same molar mass of Pd in ​​a DMF solvent, pass through a hydrogen atmosphere of hydrogen to react for 10 minutes, keep the gas atmosphere, add 3,4-difluorothiophenol as ligand M, so that M:Pd The molar ratio is 0.3:1, the stirring time is 30min, the stirring temperature is 80°C, and the M-Pd is prepared after suction filtration and drying for 12h 4 The S / X catalyst is spare (M is 3,4-difluorothiophenol).

[0060] S2: The prepared M-Pd 4 The S / X catalyst carries out semi-hydrogenation reaction with 1-phenyl-1-propyne as a substrate, and the reaction steps are: get 20ml of ethanol and transfer it to a 48ml reaction flask, get 2mmol of the substrate into the reaction flask and Ultrasonic disperse for 1 min, set the temperature to 60°C, add a corresponding amount of catalyst, the molar ratio of substrate to Pd is 2000:1, replace hydrogen 3 times and keep 1 bar of hydrogen in the reaction bottle, set the speed to 1000 rpm and turn on the stirring....

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Abstract

The invention relates to a method for preparing a catalyst, in particular to a method for preparing a catalyst obtained by modifying palladium, the catalyst and its application. In the present invention, Pd or Pd / X is modified by using a thiol ligand M to prepare M-Pd by introducing hydrogen-containing gas and maintaining the gas atmosphere. 4 S catalyst or M‑Pd 4 The S / X catalyst is modified with a relatively cheap and small amount of thiol ligands, and the prepared catalyst of the present invention has high selectivity to intermediate alkyne compounds in the alkyne semi-hydrogenation reaction, and has good reproducibility and stability The characteristics of good performance are conducive to reducing costs and widely used in industry.

Description

[0001] Technical field: the present invention relates to a preparation method of a catalyst, especially a preparation method, catalyst and application of a catalyst obtained by modifying palladium. Background technique: [0002] Selective hydrogenation of alkynes plays an important role in industrial production. Alkynes are mainly divided into two types, terminal alkynes and intermediate alkynes, especially the selective hydrogenation of intermediate alkynes in the synthesis of fine chemicals, pharmaceutical synthesis, development of health products and agricultural applications. Synthetic aspects of chemicals play an important role in catalysis, in order to obtain high yields of target products, and to make the reaction process economical, energy-saving and environmentally friendly, the development of sustainable catalysts has attracted great attention. [0003] In traditional industrial applications, in order to improve the selectivity of products, highly active metals are ge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C5/09C07C15/44
CPCB01J31/226B01J2231/645B01J2531/824C07C5/09C07C2531/22C07C15/44
Inventor 郑南峰李志恺刘圣杰陈洁
Owner XIAMEN UNIV