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A supported palladium catalyst adopting nanocarbon as a carrier, preparation thereof and applications of the catalyst

A nano-carbon and catalyst technology, applied in the field of organic catalytic reactions, can solve the problems of loss of Pd nanoparticles and long-term recycling of unfavorable catalysts, and achieve the effects of various product forms, fewer steps, and mild preparation conditions

Active Publication Date: 2015-07-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as the cross-linked HBPE repeatedly swells and shrinks during use, it is easy to cause some Pd nanoparticles to be lost, which is not conducive to the long-term recycling of the catalyst.

Method used

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  • A supported palladium catalyst adopting nanocarbon as a carrier, preparation thereof and applications of the catalyst
  • A supported palladium catalyst adopting nanocarbon as a carrier, preparation thereof and applications of the catalyst
  • A supported palladium catalyst adopting nanocarbon as a carrier, preparation thereof and applications of the catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1, comparative example 1

[0046] 1. Sample preparation

[0047] (1) Embodiment 1

[0048] Step 1: Under the protection of ethylene, inject 100 mL of anhydrous dichloromethane into a 250 mL Schlenk bottle, stir for 30 min to keep the temperature at 35 ° C; then add Pd-diimine catalyst 1 (0.2 g, previously Dissolve in 10 mL of anhydrous grade dichloromethane). After stirring the above solution at a constant polymerization temperature (35° C.) and ethylene pressure (0.1 MPa) to continue the polymerization for 24 h, the resulting product was added to 200 mL of 1% acidified methanol to terminate the polymerization. The resulting polymerized product was first purged with air to remove the solvent at room temperature, and the obtained product was dissolved in 50 mL of tetrahydrofuran (THF). particles; subsequent addition of methanol (100 mL) precipitated the polymer product. In order to further remove a small amount of catalyst ligand contained in the product, ...

Embodiment 2

[0075] Embodiment 2, comparative example 2

[0076] 1. Sample preparation

[0077] (1) Example 2

[0078] Step 1: The preparation process of HBPE is the same as Step 1 in Example 1, and the yield of HBPE is 19.7g.

[0079] Step 2: In a cylindrical glass bottle of 100mL size, add 800mg of natural flake graphite (specification is the same as described in step 2 in Example 1), 160mg HBPE (synthesized by the above step 1) and 80mL chloroform (analytical pure ), sealed and placed in a 250W ultrasonic pool for 48 hours at room temperature. The resulting product was centrifuged at 4000rpm for 45min, and about 70mL of the upper graphene solution (containing excess HBPE) was collected. Further vacuum filter the obtained graphene solution with a polytetrafluoroethylene membrane with a pore size of 0.22 μm, and rinse with fresh chloroform to remove excess HBPE, and add 30 mL of dichloromethane to the solid product after the filtration (analysis Pure), ultrasonic 8h at room temperatur...

Embodiment 3

[0103] Embodiment 3, comparative example 3

[0104] 1. Sample preparation

[0105] (1) Example 3

[0106] Step 1: The HBPE synthesis process is the same as step 1 in Example 1, and the resulting HBPE yield is 20.5 g.

[0107] Step 2: The graphene preparation process is the same as step 2 in Example 1, and a total of 60 mL of graphene solution (with chloroform as solvent, graphene concentration of 0.17 mg / mL) is obtained.

[0108] Step 3: Under the protection of nitrogen, add 42mL of the graphene solution obtained in the above step 2 (the quality of graphene is 7.14mg, and the feeding concentration is 0.12mg / mL) into a 100mL cylindrical glass bottle, and pass ultrasound at room temperature (power 250W, Time 0.5h) obtain graphene initial dispersion liquid; Further add 18mL monomer cyclopentene (13.86g, feeding concentration is 0.03mol / mg graphene) and 450mg Pd-diimine catalyst 2 (feeding concentration is 0.07 mmol / mg graphene), followed by ultrasonic (power 250W) continuous r...

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Abstract

A supported Pd catalyst adopting nanocarbon as a carrier, preparation thereof and applications of the catalyst are disclosed. The supported Pd catalyst comprises the nanocarbon carrier, a polymer covering layer on the surface of the nanocarbon carrier and Pd nano particles distributed on the surface of the polymer covering layer. The nanocarbon carrier is carbon nanotubes or graphene. The polymer covering layer is formed by polymerization of aliphatic cycloolefin on the surface of the nanocarbon carrier. The supported Pd catalyst has characteristics of mild preparing conditions, a simple process and a controllable and adjustable structure, can be used for Heck or Suzuki coupling reactions, and has advantages of high catalytic activity, easy separation and recovery, good cyclic using stability, and the like.

Description

technical field [0001] The invention relates to a supported palladium (Pd) catalyst with nano-carbon as a carrier and a preparation method and application thereof. The supported Pd catalyst can be applied to the field of organic catalytic reactions (such as Heck and Suzuki coupling reactions). Background technique [0002] Pd-based catalysts play a very important role and have broad application prospects in the field of modern organic chemistry. This type of catalyst can be used to catalyze the synthesis of various polymers, such as the coordination polymerization of olefins or olefin / CO alternating copolymerization, and can also be used to catalyze Synthesis of various small organic molecules, such as Heck and Suzuki coupling reactions. However, this type of catalyst is a precious metal resource. If the application process cannot be effectively recovered and recycled, it will not only increase the cost of use, but also cause environmental pollution problems. Therefore, how...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07B37/00C07C69/618C07C67/343C07C15/14C07C1/32C07C15/18C07C2/86
CPCY02P20/52
Inventor 徐立新钟明强孟竺
Owner ZHEJIANG UNIV OF TECH
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