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Preparation method and use of crosslinked polyethylene-loaded 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, difficult synthesis, and cumbersome preparation steps and other problems, to achieve the effect of easy separation, good stability and good chemical stability

Active Publication Date: 2013-08-28
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

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Effect test

preparation example Construction

[0016] A preparation method of cross-linked polyethylene loaded metal nanoparticles, the method is a primary load, comprising the following steps:

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

Embodiment 1

[0038] Example 1: One-step loading method synthesis of crosslinked polyethylene loaded palladium nanoparticles

[0039] In a 50mL round-bottomed flask that was dried by dehydration, it was treated by vacuum and equilibrated with ethylene. At 25°C, 5mL of palladium-diimine catalyst solution (0.1 mmol [(ArN=C(Me)-(Me)C=NAr)Pd (CH 3 ) (N≡CMe)] + SbF 6 ─ dissolved in 5 mL of dry dichloromethane), while 5 mL of 1,6-hexanediol diacrylate (0.10 g) in dichloromethane was added rapidly to start the reaction. During the reaction process, ethylene was continuously fed. 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 linked polyethylene product was swollen and crushed, and the broken cross-linked polyethylene product...

Embodiment 2

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

[0041] In a 100 mL round-bottomed flask, which was dried by removing water, and equilibrated with ethylene by vacuum treatment, at 25 °C, add 10 mL of palladium-diimine catalyst solution (0.2 mmol (ArN=C(Me)-(Me)C=NAr)Pd (CH 3 ) (N≡CMe)] + SbF 6 ─ dissolved in 10 mL of dry dichloromethane), and at the same time 10 mL of dichloromethane solution containing diene monomer bis(2-acryloyl)ethoxydisulfide (0.19 g) was added rapidly to start the reaction. During the reaction process, ethylene was continuously fed. After 24 h of reaction, 50 mL of methanol was added to the system to terminate the reaction, and a cross-linked polyethylene product was obtained. Disperse the cross-linked polyethylene product in 20 mL of dichloromethane, add 0.4 mmol of diphenyl (1,5-cyclooctadiene) platinum (II), stir and load, and react for 12 h. Then the cross-linked polyethylene produc...

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PUM

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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 nanoparticle, in particular to a preparation method of a crosslinked polyethylene-supported metal nanoparticle and an application of the crosslinked polyethylene-supported metal nanoparticle as an efficient and recyclable catalyst. Background technique [0002] Metal nanoparticles have a large specific surface area and special surface effects, which make them have high surface activity, which can effectively avoid side reactions caused by the diffusion of reactants into the particles, and 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 products will cause metal pollution. Therefore, after the catalytic reaction is completed, it is necessary to separate, recycle and reuse metal nanocatalysts. In order to facilitate the separation, recovery and reuse of catalysts, metal nanoparti...

Claims

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Application Information

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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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