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Preparation method of magnetic sulfur-containing bidentate palladium ligand catalyst

A bidentate ligand and catalyst technology, applied in the field of catalyst preparation, can solve problems such as difficulty in recovering a homogeneous palladium ligand catalyst, and achieve the effects of strong practicability and simple operation

Inactive Publication Date: 2010-06-30
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The timely problem to be solved by the present invention is to provide a preparation method of a magnetic sulfur-containing bidentate palladium ligand catalyst in order to solve the problem of difficult recovery of the existing homogeneous palladium ligand catalyst

Method used

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  • Preparation method of magnetic sulfur-containing bidentate palladium ligand catalyst
  • Preparation method of magnetic sulfur-containing bidentate palladium ligand catalyst
  • Preparation method of magnetic sulfur-containing bidentate palladium ligand catalyst

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specific Embodiment approach 1

[0007] Embodiment 1: The preparation method of the magnetic sulfur-containing bidentate palladium ligand catalyst in this embodiment is as follows: 1. Preparation of sulfur-containing bidentate ligands containing active groups: coupling sulfur-containing bidentate ligands with silane The agent is mixed according to the molar ratio of 1:1~5, stirred and heated to 40°C~110°C, then kept at 40°C~110°C for 1 hour to 8 hours, and then rotary steamed (purpose to remove excess silane coupling agent ), promptly get the sulfur-containing bidentate ligand (reaction formula as shown in (1)) containing active group; Two, Fe 3 o 4 Preparation of immobilized sulfur-containing bidentate ligands: Under the condition of inert gas protection, the sulfur-containing bidentate ligands containing active groups and superparamagnetic Fe 3 o 4 The nanoparticles are added to the solvent in turn, then ultrasonically oscillated for 20 minutes, then stirred at a temperature of 67°C to 130°C, and refluxed...

specific Embodiment approach 2

[0010] Embodiment 2: This embodiment differs from Embodiment 1 in that the sulfur-containing bidentate ligand in step 1 is 1,2-dimercaptoethane or 1,3-dimercaptopropane. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0011] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that the silane coupling agent described in step one is vinyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 3-chloropropyl Triethoxysilane, 3-bromopropyltrimethoxysilane or 3-(2,3-glycidoxy)propyltrimethoxysilane. Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a preparation method of a magnetic sulfur-containing bidentate palladium ligand catalyst, relating to a preparation method of a catalyst and solving the problem of difficult recovery of the traditional homogeneous-phase palladium ligand catalyst. The method comprises the following steps of: (1) preparing a sulfur-containing bidentate ligand containing an active group; (2) preparing a Fe3O4-immobilized sulfur-containing bidentate ligand; and (3) preparing the magnetic sulfur-containing bidentate palladium ligand catalyst to obtain the magnetic sulfur-containing bidentate palladium ligand catalyst. By adopting the preparation method, the homogeneous-phase palladium ligand catalyst is immobilized on superparamagnetic Fe3O4 nano particles, and because the superparamagnetic Fe3O4 nano particles have the characteristics that the superparamagnetic Fe3O4 nano particles can be magnetized in an external magnetic field and the magnetism disappears when the external magnetic field is removed, the magnetic sulfur-containing bidentate palladium ligand catalyst can realize the recovery of the catalyst and has the advantages of simple operation and strong practicality.

Description

technical field [0001] The invention relates to a preparation method of a catalyst. Background technique [0002] Novel methods for the synthesis of C-C bonds catalyzed by transition metals have always been a research hotspot in the field of catalysis. Especially in 1979, Suzuki et al. reported the C-C bond synthesis reaction involving organoboron reagents (called Suzuki-Miyaura coupling reaction), which opened up a new path for the field of green chemistry. In recent years, the Suzuki-Miyaura coupling reaction has been widely used in biomedicine, electronic devices, synthesis of display materials and other fields. Most of the Suzuki-Miyaura coupling reaction is carried out under the homogeneous palladium ligand catalyst, the homogeneous palladium ligand catalyst has high catalytic efficiency and good selectivity, but the recovery of the existing homogeneous palladium ligand catalyst is difficult, which increases the cost of use. Therefore, its wide application is limited....

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C205/06C07C201/12C07C253/30C07C255/50C07C45/68C07C47/546C07C49/784C07B37/04
Inventor 白雪峰王亮樊慧娟吕宏飞
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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