Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of single-atom palladium catalyst and its application in carbon-carbon coupling

A palladium catalyst and atomic technology, applied in the field of catalysts, can solve the problems of no zero-valent single-atom palladium catalyst reports, etc., and achieve the effect of highly efficient catalytic carbon-carbon coupling reaction

Active Publication Date: 2022-07-15
SHAOXING UNIVERSITY +1
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the preparation technology, there is no report on the zero-valent monoatomic palladium catalyst

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of single-atom palladium catalyst and its application in carbon-carbon coupling
  • Preparation method of single-atom palladium catalyst and its application in carbon-carbon coupling

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0024] The present invention provides a Pd 0 / Pd 2+ Preparation method of ratio-adjustable single-atom palladium catalyst and its application in carbon-carbon coupling. The Pd 0 / Pd 2+ The preparation method of the ratio-adjustable single-atom palladium catalyst comprises: firstly dispersing metal palladium salt and titanium dioxide on the surface of graphene oxide uniformly; then, illuminating the above mixture under stirring conditions, thereby forming palladium monolayers of different valences on the surface of the carrier. atom. Finally, after washing and freeze-drying operations, single-atom palladium catalysts with different valence states are obtained.

[0025] In a preferred embodiment, the preparation method comprises the following steps:

[0026] 1. Evenly mix palladium salt, titanium dioxide, graphene oxide and dehydrated alcohol in a mass ratio of 1:1~20:1~50:1000 to obtain solution A;

[0027] 2. Under the stirring speed of 1~2000r / min, the solution A is irr...

Embodiment 1

[0036] 7.5 mg of potassium chloropalladate, 50 mg of brookite-type titanium dioxide, 1.5 mg of graphene oxide and 35 ml of absolute ethanol were added to a beaker, and the solution was uniformly dispersed by ultrasonic for 5 minutes to obtain solution A1.

[0037] The solution A1 was reacted for 12 hours at a stirring speed of 2000 r / min under the illumination of 400 nm to obtain a solution B1.

[0038] The solution B1 was filtered, the filter cake was washed three times with ethanol and water, and the filter cake was freeze-dried at -60°C for 48 hours to prepare Pd 0 / Pd 2+ Monoatomic palladium content (by metal mass) as 0.4% of the carrier, Pd 0 / Pd 2+ A ratio of 8% single-atom palladium catalyst C1.

[0039] Add 4-iodoacetophenone (400mg), phenylboronic acid (300mg), catalyst C10.5mg, potassium phosphate 280mg to a 100ml three-necked flask, heat to 100°C, react for 10min, and detect the reaction process in liquid phase to obtain the target The product liquid phase yield...

Embodiment 2

[0041] 10 mg of palladium chloride, 60 mg of anatase titanium dioxide, 1.2 mg of graphene oxide and 35 ml of absolute ethanol were added to a beaker, and the solution was uniformly dispersed by ultrasonic for 5 minutes to obtain solution A2.

[0042] The solution A2 was reacted for 24 hours at a stirring speed of 1000 r / min under the illumination of 400 nm to obtain a solution B2.

[0043] The solution B2 was filtered, the filter cake was washed three times with ethanol and water, and the filter cake was freeze-dried at -60°C for 48 hours to prepare Pd 0 / Pd 2+ Monoatomic palladium content (by metal mass) as 0.3% of the carrier, Pd 0 / Pd 2+The proportion of 15% single atom palladium catalyst C2.

[0044] Add 4-iodoacetophenone (400mg), phenylboronic acid (300mg), catalyst C20.5mg, potassium phosphate 280mg to a 100ml three-necked flask, heat to 100°C, react for 10min, and detect the reaction process in liquid phase to obtain the target The product liquid phase yield was 72...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention provides a preparation method of a single-atom palladium catalyst and its application in carbon-carbon coupling, wherein the single-atom palladium catalyst is Pd 0 / Pd 2+ The single-atom palladium catalyst with adjustable ratio, the preparation method comprises: firstly dispersing metal palladium salt and titanium dioxide on the surface of graphene oxide; single atom. Finally, after washing and freeze-drying operations, a Pd 0 / Pd 2+ A ratio-tunable single-atom palladium catalyst. Pd prepared by the present invention 0 / Pd 2+ The ratio-tunable single-atom palladium catalyst can efficiently catalyze the carbon-carbon coupling reaction.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a kind of Pd 0 / Pd 2+ Preparation method of ratio-adjustable single-atom palladium catalyst and its application in carbon-carbon coupling. Background technique [0002] Palladium-catalyzed carbon-carbon coupling reaction is one of the important methods to construct C-C bonds and plays an important role in drug synthesis. However, due to the shortage of palladium catalysts such as low reserves and high price, it is of great significance to develop new and recyclable high-efficiency palladium catalysts for carbon-carbon coupling reactions. [0003] At present, a large number of heterogeneous palladium catalysts have been continuously prepared and reported, which greatly improves the efficiency of carbon-carbon coupling reactions, but there are still great challenges to further improve their catalytic efficiency. Single-atom catalysts have become a major research hotspot due to...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07C45/68C07C49/784
CPCB01J23/44C07C45/68C07C49/784
Inventor 杜奎盛力范钢吴旭锋钱武蒙利民沈润溥
Owner SHAOXING UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com