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Preparation method and application of graphene-oxide-loaded diimine-coordinated palladium

A diimine ligand and diimine technology, which is applied in the preparation of organic compounds, carbon-based compounds, chemical instruments and methods, etc., can solve the problems of easy agglomeration failure, easy loss of palladium, low catalytic activity, etc.

Active Publication Date: 2019-10-08
GUANGDONG PHARMA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the problems in the prior art that ordinary heterogeneous palladium catalysts are prone to agglomeration and failure, the catalytic activity is not high, the palladium of homogeneous coordination palladium catalysts is easy to lose, and the post-treatment of products is difficult. One of the purposes of the present invention is to provide an oxidation Graphene supported diimine coordination palladium, the second purpose of the present invention is to provide the preparation method of this graphene oxide supported diimine coordination palladium, the third purpose of the present invention is to provide this graphene oxide supported diimine coordination palladium. Application of amine-coordinated palladium

Method used

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  • Preparation method and application of graphene-oxide-loaded diimine-coordinated palladium
  • Preparation method and application of graphene-oxide-loaded diimine-coordinated palladium
  • Preparation method and application of graphene-oxide-loaded diimine-coordinated palladium

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Experimental program
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Embodiment

[0077] 1. Preparation of Graphene Oxide

[0078] 23mL of concentrated sulfuric acid (98wt%H 2 SO 4 ), cooling in an ice bath to ensure that the system temperature is lower than 5°C, add 1g of graphite powder under stirring, and continue stirring for 1h. After mixing well, slowly add 3g KMnO 4 , in order to prevent liquid splashing, the reaction temperature needs to be controlled below 20°C (stirring and dropping speed is slow and uniform), and react for 1h. Place the beaker in a constant temperature water bath at 35°C, stir evenly, and react for 3 hours. Add 46mL of deionized water, (slowly, along the wall, exothermic) control the reaction temperature to 95°C, keep stirring for 15min, then add 140mL of water to stop the reaction. 5mL hydrogen peroxide (30wt%H 2 o 2 ) into the reaction system (first fast and then slow), stop when the solution just turns yellow, the solution turns from brown-black to bright yellow, pour off the supernatant, wash 2 times with 2wt% HCl solut...

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Abstract

The invention discloses a preparation method of graphene-oxide-loaded diimine-coordinated palladium, and application of the graphene-oxide-loaded diimine-coordinated palladium serving as a catalyst inorganic synthesis reactions. The preparation method of the graphene-oxide-loaded diimine-coordinated palladium includes the following steps: 1) reacting aldehyde-containing diimine with a silane coupling agent to obtain a silane coupling agent modified diimine ligand, 2) reacting the silane coupling agent modified diimine ligand with graphene oxide to obtain a graphene-oxide-loaded diimine ligand; 3) reacting the graphene-oxide-loaded diimine ligand with a palladium salt. The obtained catalyst can efficiently catalyze Suzuki coupling reactions and direct C-H arylation reactions at a very lowdosage; the ligands are firmly loaded on graphene by Schiff base bonding, and accordingly, the catalyst can be recycled for many times and has good application and promotion prospects.

Description

technical field [0001] The invention belongs to the technical field of catalytic materials, and in particular relates to a preparation method and application of graphene oxide-loaded diimine-coordinated palladium. Background technique [0002] Palladium is located in the second transition period. Its moderate atomic radius and unique electron arrangement form the stability of the palladium complex and the diversity of its catalytic performance, especially for the reactions involving the formation of carbon-carbon bonds. It has outstanding catalytic activity. . Homogeneous catalysts such as palladium salts and palladium complexes were widely used at first, which have the advantages of good dispersion, high catalytic efficiency, and excellent selectivity. However, because the catalyst and the reaction system react in the same phase, it is difficult to separate the catalyst and expensive Palladium is not only difficult to recycle, but also remains to pollute the product. Ther...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C249/02C07C251/08C07F15/00C07F7/18C07C45/68C07C47/546C07C47/575C07C49/782C07C49/84C07C67/343C07C1/32C07C69/78C07C15/14C07C17/263C07C25/18C07C41/30C07C43/205C07C253/30C07C255/50C07C255/54C07C201/12C07C205/06C07D277/22C07D277/24C07D277/30
CPCC07C249/02C07C251/08C07F15/0066C07F7/1804C07F7/1892B01J31/1805C07C45/68C07C67/343C07C1/321C07C17/263C07C41/30C07C253/30C07C201/12C07D277/22C07D277/24C07D277/30B01J2531/0241B01J2531/824C07C47/546C07C47/575C07C49/782C07C49/84C07C69/78C07C15/14C07C25/18C07C43/205C07C43/2055C07C255/50C07C255/54C07C205/06Y02P20/584
Inventor 李田孙云龙刘丰收
Owner GUANGDONG PHARMA UNIV
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