Preparation method of palladium catalyst, catalyst and application

A palladium catalyst and a catalyst technology are applied in the field of preparation of palladium catalysts, which can solve the problems of difficult industrial-scale application production, increase the use of precious metals, and low utilization rate of palladium, and achieve good reproducibility, low price, and industrial application. Effect

Inactive Publication Date: 2020-11-10
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent No. 128595 discloses a method, adding alkyne-containing gas vapor and an inert hydrocarbon solvent into a reaction vessel to carry out catalytic hydrogenation with a VIII group metal-alumina catalyst such as palladium, nickel, etc., but the alkyne-containing gas Poor solubility in hydrocarbon solvents; patent CN101428228A discloses a selective hydrogenation catalyst, wherein the active component of the catalyst is palladium, auxiliary agent copper, and alumina is used as a carrier, and the catalyst is suitable for rich in alkyne residues Selective hydrogenation to remove alkyne, its carrier treatment and preparation need high temperature above 900°C for treatment
[0004] Due to the high activity of palladium, the site of poisoning part is often needed to have good selectivity to alkynes, which leads to the low utilization rate of palladium, increases the use of precious metals, and increases the cost; on the other hand, The preparation method of selective semi-hydrogenation catalyst, especially the preparation method of selective semi-hydrogenation catalyst for terminal alkynes is relatively complicated, and it is difficult to carry out industrial-scale application production

Method used

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  • Preparation method of palladium catalyst, catalyst and application
  • Preparation method of palladium catalyst, catalyst and application
  • Preparation method of palladium catalyst, catalyst and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1: palladium nanosheet preparation catalyst carries out semi-hydrogenation reaction

[0046] S1: choose two-dimensional palladium nanosheets (Pd Ns) dispersed in ethanol solvent, add triphenylphosphine sulfur (PPh 3 S) As modifier H, the molar ratio of modifier H:Pd is 1:0.4, the stirring time is 1 h, the stirring temperature is 20°C, the catalyst is filtered out with suction, washed and dried with ultrapure water for 12 h to prepare PPh 3 S-Pd Ns catalyst.

[0047] S2: The prepared PPh 3The S-Pd Ns catalyst uses phenylacetylene as a substrate for semi-hydrogenation reaction. Reaction steps: transfer 20ml of ethanol solvent to a 48ml reaction flask, select 2mmol of phenylacetylene into the reaction flask and ultrasonically disperse for 1min, set the temperature to 30°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 rotation speed to 10...

Embodiment 2

[0049] S1: Disperse Pd / C with a Pd mass fraction of 5% in ethanol solvent, add triphenylphosphine sulfur (PPh 3 S) As modifier H, the molar ratio of modifier H:Pd is 1:0.25, the stirring time is 1 h, the stirring temperature is 30°C, the catalyst is filtered out with suction, washed and dried with ultrapure water for 12 h to prepare PPh 3 The S-Pd / C catalyst is ready for use.

[0050] S2: The prepared PPh 3 The S-Pd / C catalyst uses phenylacetylene as a substrate for semi-hydrogenation reaction. Reaction steps: transfer 20ml of ethanol to a 48ml reaction flask, select 2mmol of phenylacetylene into the reaction flask and ultrasonically disperse it for 1min, set the temperature to At 30°C, add a corresponding amount of catalyst, the molar ratio of substrate to Pd is 2000:1, replace hydrogen 3 times and keep 1bar of hydrogen in the reaction bottle, set the rotation speed to 1000rpm and turn on the stirring. Timely sampling is carried out the detection of product by gas chromatog...

Embodiment 3

[0051] Embodiment 3: test the stability of catalyst of the present invention

[0052] S1: Select Pd / C with a Pd mass fraction of 5% and disperse it in an ethanol solvent, add triphenylphosphine sulfur (PPh 3 S) As modifier H, the molar ratio of modifier H:Pd is 1:0.4, the stirring time is 1h, the stirring temperature is 25°C, the catalyst is filtered out with suction, washed and dried with ultrapure water for 12h to prepare PPh 3 S-Pd / C catalyst.

[0053] S2: The prepared PPh 3 The S-Pd / C catalyst uses phenylacetylene as a substrate for semi-hydrogenation reaction. Reaction steps: transfer 20ml of ethanol to a 48ml reaction flask, select 2mmol of phenylacetylene into the reaction flask and ultrasonically disperse it for 1min, set the temperature to 30°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 rotation speed to 1000rpm and turn on the stirring. ...

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Abstract

The invention provides a preparation method of a palladium catalyst, the catalyst and application. The catalyst is prepared by directly using aromatic compounds containing phosphorus and sulfur substituents, such as triphenylphosphine sulfur, diphenyl phosphorus hydrosulfide and the like, as modifiers to modify Pd or Pd/X with a carrier. The amount of modifiers for preparing the catalyst is low and the preparation method is simple and convenient; the prepared catalyst has efficient and stable catalytic activity and can be used for alkyne semi-hydrogenation reaction, wherein high selectivity isachieved on terminal alkyne compound semi-hydrogenation, and industrial application is facilitated.

Description

[0001] Technical field: the present invention relates to a kind of preparation method of catalyst, particularly a kind of preparation method of palladium catalyst, catalyst and application. Background technique: [0002] Cracking to olefins has a very wide range of uses in the petrochemical industry and occupies a very important position. However, there will be trace amounts of alkynes and dienes while producing corresponding olefins. Although the content of these alkynes and dienes is small, they will affect the polymerization effect of olefins and reduce the quality of the product. Therefore, it is necessary to remove these trace impurities remove. Commonly used methods in industry include solvent absorption, low-temperature rectification, and selective hydrogenation to remove the corresponding alkynes. It is a relatively simple and convenient method to catalytically hydrogenate the corresponding alkynes to form alkenes by catalytic hydrogenation. However, alkenes can be ea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J27/232B01J23/63B01J31/26B01J31/02C07B35/02C07C5/09C07C15/46C07C11/02C07C209/70C07C211/45C07D213/127C07D213/16
CPCB01J23/44B01J23/63B01J27/232B01J31/0267B01J31/0271B01J31/26B01J2231/645C07B35/02C07C5/09C07C209/70C07D213/127C07D213/16C07C15/46C07C11/02C07C211/45
Inventor 郑南峰荆文彤李志恺刘圣杰陈洁
Owner XIAMEN UNIV
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