Core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst

A nitrogen heterocyclic carbene, core-shell structure technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, carbon-based compound preparations, etc., can solve problems such as improvement and unfavorable industrial benefits, Achieve the effect of high catalytic activity, reduced industrial cost, and high industrial application value

Inactive Publication Date: 2015-01-28
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, many current magnetic spherical catalysts are made by grafting functional groups onto magnetic nano-cores. The whole grafting process often has to go through a series of cumbersome processes, which is not conducive to the improvement of industrial benefits.

Method used

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  • Core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst
  • Core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst
  • Core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst

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Experimental program
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Effect test

Embodiment 1

[0015] Embodiment 1 (catalyst Fe 3 o 4 Preparation and application of PNP1)

[0016] Dissolve 100 mg of palladium acetate in 10 mL of DMF solution, then add 210 mg of TIPT-Cl and Fe containing imidazolium salt under ultrasonication 3 o 4 Nanoparticles in 70mL DMF solution, and then the reaction system was reacted at 90°C for 1h under ultrasonic conditions, and then reacted at 110°C in an oil bath for 5h. After the reaction was completed, cooled to room temperature, and the obtained solid was collected and separated under an external magnetic field. , and then washed several times with DMF, dichloromethane and ether, and then dried under vacuum to obtain the magnetic spherical catalyst Fe 3 o 4 PNP1.

[0017] Catalyst Fe 3 o 4 The content of Pd in ​​PNP1 is 1.07mmol / g and the thermal stability is at least above 250°C.

[0018] Catalyst Fe 3 o 4 PNP1 is used in the Suzuki coupling reaction of 4-bromoacetophenone and phenylboronic acid, the catalyst dosage is 1%, the re...

Embodiment 2

[0019] Embodiment 2 (catalyst Fe 3 o 4 Preparation and application of PNP2)

[0020] Dissolve 100mg of palladium acetate in 10mL of DMF solution, then add to the solution containing 210mg of imidazolium salt TIPB-Cl and appropriate amount of Fe 3 o 4 Nanoparticles in 70mL DMF solution, and then the reaction system was reacted under ultrasonic at 90°C for 1h, and then reacted in an oil bath at 110°C for 5h. After the reaction was completed, cooled to room temperature, the obtained solid was Collect and separate, then wash several times with DMF, dichloromethane and ether, then dry under vacuum to obtain the magnetic spherical catalyst Fe 3 o 4 PNP2.

[0021] Catalyst Fe 3 o 4 The content of Pd in ​​PNP2 is 0.82mmol / g, and the thermal stability is at least 250℃.

[0022] Catalyst Fe 3 o 4 PNP2 is used for the Suzuki coupling reaction of 4-bromoacetophenone and phenylboronic acid, the catalyst dosage is 1%, the reaction temperature is room temperature, the reaction time...

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Abstract

The invention discloses a core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst and a preparation method thereof and belongs to the technical field of organometallic polymers. The core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst comprises a paramagnetic Fe3O4 core and a precious metal-nitrogen heterocyclic Carbene polymer coating the surface of the paramagnetic Fe3O4 core. In the presence of Fe3O4 nano-particles, an imidazolium salt monomer TIPT-Cl or TIPB-Cl and a precious metal acetate undergo an ultrasonic reaction at a temperature of 90 DEG C in N,N-dimethyl formamide (DMF) as a solvent for 1h, and then the reaction system undergoes a reaction in an oil bath at a temperature of 110 DEG C for 5h to product the core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst. The core-shell structure precious metal-nitrogen heterocyclic Carbene polymer magnetic catalyst has high-dispersed active sites and good catalytic activity. Through the magnetic Fe3O4 core, the catalyst can be separated easily in the liquid phase reaction and can be conveniently recovered and recycled.

Description

technical field [0001] The invention relates to the preparation of a magnetic nanoparticle catalyst wrapped with a noble metal nitrogen heterocyclic carbene palladium polymer and its application in a liquid-phase catalytic reaction, belonging to the technical field of metal organic compounds. Background technique [0002] Nano- and micro-scale spherical particles have attracted more and more attention in the fields of catalysis, drug delivery and materials science. Among them, the metal-organic coordination polymer particle is a kind of spherical material with wide application prospect, and this polymer is formed by the direct coordination of metal ions and organic ligands of multi-coordinating groups. Compared with traditional functionalized metal-organic compounds, azacarbene metal-organic polymers have unique advantages in heterogeneous catalysis: for example, carbene has a strong electron-donating ability to metal atoms, which can improve the activity of the catalyst; O...

Claims

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Application Information

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IPC IPC(8): B01J31/28C07B37/00C07C45/68C07C49/782
Inventor 赵怀霞王瑞虎
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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