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Loaded palladium catalyst, its preparation method and application

A technology of supported palladium and catalyst, applied in the field of supported palladium catalyst and its preparation and application, which can solve the problems of low catalytic activity, difficult recovery, complicated preparation method, etc., and achieve the effects of high activity, easy operation and simple preparation method

Inactive Publication Date: 2013-12-18
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still many shortcomings in the industrial application of palladium catalysts, which greatly limit the performance and application of palladium catalysts.
Although the preparation process of the palladium-carbon catalyst is simple, the loading capacity of palladium cannot be adjusted well, and the catalytic activity is low; the palladium coordination catalyst has high activity, but the preparation method is complicated, the catalytic environment is harsh, and it is difficult to recycle.

Method used

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  • Loaded palladium catalyst, its preparation method and application
  • Loaded palladium catalyst, its preparation method and application
  • Loaded palladium catalyst, its preparation method and application

Examples

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preparation example Construction

[0012] The preparation method of the supported palladium catalyst of the present invention comprises that polyethynyl aromatic compound is contacted with tetrakis (triphenylphosphine) palladium and / or dichlorobis (triphenylphosphine) palladium in an organic solvent, and The contacted product is subjected to solid-liquid separation to obtain a supported palladium catalyst; the polyethynyl aromatic compound, the total amount of tetrakis (triphenylphosphine) palladium and dichlorobis (triphenylphosphine) palladium The molar ratio is 3-30:1.

[0013] According to the present invention, the polyethynyl aromatic compound and the usage amount of the tetrakis(triphenylphosphine)palladium and / or dichlorobis(triphenylphosphine)palladium can be obtained according to the expected supported palladium The loading amount of palladium element of the catalyst is properly selected. Preferably, the molar ratio of the polyethynyl aromatic compound to the total amount of tetrakis(triphenylphosphi...

Embodiment 1

[0040] This example is used to illustrate the preparation of supported palladium catalyst.

[0041] In a 20 ml four-neck flask equipped with a reflux tube and a thermometer, add 150 mg of 1,3,5-triethynylbenzene (purchased from Alfa Aisha (Tianjin) Company, with a purity of 98% by weight, the same below), 115.5 mg of tetrakis(triphenylphosphine) palladium (purchased from Alfa Aisha (Tianjin) Co., with a purity of more than 99% by weight, the same below) and 5 ml of tetrahydrofuran were stirred to make 1,3,5-triethynyl After benzene and tetrakis(triphenylphosphine)palladium were completely dissolved, they were reacted at 65°C for 12 hours, and the solid was separated, washed twice with 3 ml of ethanol, and then vacuum-dried at 80°C for 12 hours to obtain supported palladium catalyst. The transmission electron micrograph of this loaded palladium catalyst is as follows figure 1 said, through figure 1 It can be seen that the supported palladium catalyst is a palladium particle ...

Embodiment 2

[0043] This example is used to illustrate the preparation of supported palladium catalyst.

[0044] In a 20 ml four-neck flask equipped with a reflux tube and a thermometer, add 300 mg of 1,4-diethynylbenzene (purchased from Aladdin Company, with a purity of 97% by weight), 115.5 mg of tetrakis(triphenylphosphine) Palladium and 10 ml of tetrahydrofuran, under stirring to completely dissolve 1,4-diethynylbenzene and tetrakis(triphenylphosphine)palladium, react at 80°C for 5 hours, separate the solid, and wash with 3 ml of ethanol 2 times, and then vacuum-dried at 80° C. for 12 hours to obtain a supported palladium catalyst. The transmission electron microscope photo of the supported palladium catalyst shows that the supported palladium catalyst is a structure in which palladium particles are wrapped in polymers, and the average particle size of the palladium metal particles is about 5 nanometers; it can be seen from the infrared absorption spectrum of the supported palladium ca...

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Abstract

The invention discloses a loaded palladium catalyst, its preparation method and application. The preparation method of the catalyst comprises: contacting a polyethynyl aromatic compound with tetrakis(triphenylphosphine)palladium and / or dichloro-bis(triphenylphosphine)palladium in an organic solvent, and subjecting the contact product to solid-liquid separation, thus obtaining the loaded palladium catalyst. The polyethynyl aromatic compound and the total of the tetrakis(triphenylphosphine)palladium and the dichloro-bis(triphenylphosphine)palladium are in a molar ratio of 3-30:1. The loaded palladium catalyst prepared by the method disclosed in the invention has the advantages of simple preparation method, easy operation, easy control of the palladium load and the like. The prepared loaded palladium catalyst can be used for coupling reaction catalysis, can have high catalytic activity, and can be used repeatedly.

Description

technical field [0001] The invention relates to a supported palladium catalyst and its preparation method and application. Background technique [0002] Catalysis industry, as one of the pillar industries of chemical industry and even modern human civilization, has been paid more and more attention by people. All over the world, countries have invested a lot of human and financial resources in improving existing catalysts and developing catalysts with higher performance. Platinum, palladium, rhodium, silver, ruthenium and other noble metal catalysts, as the most important catalyst materials, have become a hot spot in the research of catalytic materials because of their comprehensive excellent properties such as high catalytic activity, high temperature resistance, oxidation resistance, and corrosion resistance. . [0003] Palladium catalyst, as a kind of noble metal catalyst, is widely used in the fields of electrocatalysis, hydrogenation reduction and coupling reaction. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07B37/00C07C15/14C07C1/32C07C49/784C07C45/68C07C205/06C07C201/12C07C43/205C07C41/30C07C33/24C07C29/32C07C15/24C07C39/15C07C37/18C07C69/767C07C67/343
Inventor 智林杰宋琪罗彬梁明会贾玉莹郝龙
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA