Loaded aurum palladium catalyst and preparation method and application thereof

A catalyst and supported technology, which is applied to the supported gold-palladium catalyst and its preparation and application fields, can solve the problems of harsh reaction conditions, poisoning, loss of reactive components, etc., and achieve excellent recycling performance and high catalytic activity. Effect

Active Publication Date: 2012-12-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many problems in the traditional reaction process: 1. Using organic solvents and using a large amount of phosphorus-containing ligands, the reaction conditions are relatively harsh; 2. Using homogeneous palladium catalysts
The catalyst has high activity for chlorobenzene Suzuki Cross-coupling in aqueous solution, but the disadvantage is that the mercapto group in the carrier has a certain poisoning effect on gold nanoparticles, and there is a certain loss of reactive components

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take a certain amount of 717 resin and dry it naturally at room temperature, weigh 5g of the dried resin, and ball mill it in a planetary ball mill at a speed of 200r / h for 3 hours. Sieve the ball-milled resin, and get the particles with 100-200 mesh for later use. The sieved resin was successively mixed with mass concentration 4% NaOH, mass concentration 5% HCl, 1mol / L Na 2 CO 3 Wash for 6 hours, and wash with deionized water until neutral after each wash. Finally, it was washed with absolute ethanol and dried under vacuum at 60°C. Weigh 1g of resin powder into 300mL ultrapure water, add 0.68mL9.56mg under stirring Au / mL HAuCl 4 solution and 0.29mL 12.00mg Pd / mL H 2 PdCl 4 The solution was stirred at room temperature for 1 h. After suction filtration, disperse the filter cake in 300mL ultrapure water, add 0.68mL9.56mg Au / mL HAuCl 4 solution and 0.29mL 12.00mg Pd / mL H 2 PdCl 4The solution was stirred for 1 h. Suction filter and wash with 500mL ultrapur...

Embodiment 2

[0035] Example 2: Weigh 1g of resin powder in 300mL of ultrapure water, add 1.36mL of 9.56mg under stirring Au / mL HAuCl 4 The solution was stirred at room temperature for 1 h. After suction filtration, disperse the filter cake in 300mL ultrapure water, add 0.58mL 12.00mg Pd / mL H 2 PdCl 4 The solution was stirred for 1 h. Suction filter and wash with 500mL ultrapure water. Disperse the filter cake in 30 mL of ultrapure water, add 20 mL of 0.065 mol / L sodium borohydride solution at one time under stirring, and continue stirring for 1.5 h. Filter with suction, wash the catalyst with 400 mL of ultrapure water and 20 mL of absolute ethanol in sequence, and dry in vacuum at 60°C for 12 hours. A catalyst with Au / Pd=1 / 1 with a loading of 2wt% can be obtained, which is designated as 2# catalyst.

[0036] Electron microscope analysis shows that the particle size of the Au-Pd nanoparticles is about 3.0 nm, and the particle size is small and uniformly dispersed.

Embodiment 3

[0037] Example 3: Weigh 1g of resin powder in 300mL of ultrapure water, add 0.33mL of 9.56mg under stirring Au / mL HAuCl 4 solution and 0.57mL 12.00mg Pd / mL H 2 PdCl 4 solution, ion exchange at room temperature for 1 h. Repeat the ion exchange once after suction filtration. Wash the filter cake with 500mL of ultrapure water and disperse it in 30mL of ultrapure water, add 20mL of 0.08mol / L sodium borohydride solution at one time, react with suction for 1.5h, and wash the catalyst with 400mL of ultrapure water and 20mL of absolute ethanol And vacuum dried at 60°C for 12h. A catalyst with Au / Pd=1 / 4 with a loading of 2wt% can be obtained, which is designated as 3# catalyst.

[0038] Electron microscope analysis shows that the particle size of the Au-Pd nanoparticles is about 2.5 nm, and the particle size is small and uniformly dispersed.

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Abstract

The invention relates to a loaded aurum palladium catalyst for coupling benzene chloride in an aqueous solution. According to the loaded aurum palladium catalyst, active components comprise Au and Pd, and a carrier is ionic exchange resin, wherein the content of the active components is 0.1 to 5 weight percent, aurum and palladium form an alloy, the grain diameter is 1 to 6 nanometers, and the relative molar ratio of aurum to palladium is 1 / 6-6 / 1. A preparation method comprises the following processes of: performing ionic exchange on resin which is subjected to ball-milling and sieving and a metal precursor; and reducing loaded metal precursor. The catalyst is used for Ullmann Reaction and Suzuki Cross-coupling in the aqueous solution, and has high catalytic performance. The catalyst is easy to prepare, and has high catalytic activity and stability.

Description

technical field [0001] The invention relates to a supported gold-palladium catalyst, a preparation method thereof and an application in coupling reaction of chlorobenzene in aqueous solution. Background technique [0002] Gold has long been considered a catalytically inert metal. Since Haruta discovered in 1987 that highly dispersed gold nanoparticles supported by oxides can efficiently catalyze the low-temperature oxidation of CO, expanding the catalytic performance of gold nanoparticles has gradually become a research hotspot in the field of catalysis. Nano-gold catalysts have shown excellent catalytic activity and selectivity in some liquid-phase organic reactions such as alcohol oxidation, amine oxidation, nucleophilic addition of unsaturated hydrocarbons, and C-C coupling reactions. [0003] Suzuki Cross-coupling is an important C-C coupling reaction of aromatic hydrocarbons, and its product biphenyl and its derivatives have important applications in alkaloids, chiral ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C15/14C07C1/32
Inventor 张磊磊王爱琴张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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