Preparation method and application of cross-linked polyethylene supported metal nanoparticles

A technology of metal nanoparticles and cross-linked polyethylene, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, bulk chemical production, etc., can solve high cost, cumbersome preparation steps, and difficult synthesis and other problems, to achieve the effect of easy separation, good stability and good chemical stability

Active Publication Date: 2016-01-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing reports on the preparation of cross-linked polymer-supported metal nanoparticle catalysts all have problems such as cumbersome preparation steps, difficult synthesis, and high cost. The patent reports of cross-linked polymers used as carriers are limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0016] A method for preparing cross-linked polyethylene loaded metal nanoparticles, the method is one-time loading, and includes the following steps:

[0017] 1. One-time support synthesis of cross-linked polyethylene loaded with palladium metal nanoparticles: use palladium-diimine catalyst to perform ethylene and diene monomers and / or functions in a dried organic solvent at -30~50℃ The "one-pot" copolymerization of monomers, in which the palladium-diimine catalyst concentration is 0.001-1mol / L, the diene monomer concentration is 0.01-2mol / L, the functional monomer concentration is 0.01-2mol / L, and the ethylene The pressure is 0.1-100atm, and the reaction time is 0.5-48h; in the polymerization process, before the polyethylene gel is formed, palladium salt is added, and the concentration of the palladium salt is 0-5mol / L. After the reaction is completed, a reaction terminator is added, and the volume ratio of the reaction terminator to the organic solvent is 1-100:1 to obtain a cr...

Embodiment 1

[0038] Example 1: One-step synthesis of cross-linked polyethylene supported palladium nanoparticles

[0039] A 50mL round-bottomed flask dried with water removed, vacuum treated and equilibrated with ethylene, and 5mL of palladium-diimine catalyst solution (0.1mmol[(ArN=C(Me)-(Me)C=NAr)Pd (CH 3 )(N≡CMe)] + SbF 6 ─ Dissolve in 5 mL of dry dichloromethane), and at the same time add 5 mL of a dichloromethane solution containing 1,6-hexanediol diacrylate (0.10 g) quickly to start the reaction. During the reaction, the continuous feeding of ethylene was maintained. After 24 hours of reaction, 40 mL of methanol was added to the system to terminate the reaction to obtain a cross-linked polyethylene product. The cross-linked polyethylene product was washed three times with 40 mL of methanol, and then the cross-linked polyethylene product was washed with 40 mL of tetrahydrofuran. The ethylene product was swelled and crushed, and the crushed cross-linked polyethylene product was washed th...

Embodiment 2

[0040] Example 2: Two-step support method synthesis of cross-linked polyethylene supported platinum nanoparticles

[0041] A 100mL round-bottomed flask dried with water removed, vacuum treated and equilibrated with ethylene, and 10mL of palladium-diimine catalyst solution (0.2mmol(ArN=C(Me)-(Me)C=NAr)Pd( CH 3 )(N≡CMe)] + SbF 6 ─ Dissolved in 10 mL of dry dichloromethane), while adding 10 mL of diene monomer bis(2-acryloyl)ethoxydisulfide (0.19g) in dichloromethane solution quickly to start the reaction. During the reaction process, continuous feeding of ethylene was maintained. After 24 hours of reaction, 50 mL of methanol was added to the system to terminate the reaction to obtain a cross-linked polyethylene product. The cross-linked polyethylene product was dispersed in 20 mL of dichloromethane, 0.4 mmol of diphenyl (1,5-cyclooctadiene) platinum (II) was added, and the mixture was stirred for loading and reacted for 12 h. Then the cross-linked polyethylene product was washed ...

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Abstract

The invention discloses a preparation method and a use of crosslinked polyethylene-loaded metal nanoparticles. The preparation method comprises that ethylene and a crosslinking monomer undergo a chain walking copolymerization reaction in the presence of a palladium-diimine catalyst to produce a crosslinked polyethylene carrier for loading metal nanoparticles; through a one-step loading or two-step loading technology, a metal compound is fixedly loaded on the crosslinked polyethylene carrier; and the metal compound loaded by the crosslinked polyethylene carrier undergoes a reduction reaction and is transformed into metal nanoparticles so that the crosslinked polyethylene-loaded metal nanoparticle catalyst is obtained. The crosslinked polyethylene-loaded metal nanoparticles are used for catalysis of a carbon-carbon cross-coupling reaction, has high catalytic activity and good stability, and can be recovered and recycled easily.

Description

Technical field [0001] The invention relates to a metal nano particle, in particular to a preparation method of a cross-linked polyethylene supported metal nano particle and the application of the cross-linked polyethylene supported metal nano particle as a highly efficient recyclable catalyst. Background technique [0002] Metal nanoparticles have a large specific surface area and special surface effects, which make them have high surface activity. They can effectively avoid side reactions caused by the diffusion of reactants into the particles. They have high activity and selectivity. Therefore, It is widely used as a catalyst for organic chemical reactions. [0003] Due to the high cost of metals, especially precious metals, residues in the products will cause metal pollution. Therefore, after the catalytic reaction is completed, the metal nano-catalyst needs to be separated, recovered and reused. In order to facilitate the separation, recovery and reuse of the catalyst, metal ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C08F210/02C08F222/14C08F216/36C08F4/80
CPCY02P20/52
Inventor 王文俊刘平伟叶志斌李伯耿
Owner ZHEJIANG UNIV
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