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Supported catalyst and application thereof in preparing telechelic low-molecular-weight poly(phenylene oxide)

A low-molecular-weight, polyphenylene ether technology, used in chemical recycling and other directions, can solve the problems of difficult separation and reduced catalytic efficiency, and achieve the effects of easy control, simple operation and high catalytic efficiency.

Active Publication Date: 2020-03-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the catalysts for the synthesis of polyphenylene ether are still mainly homogeneous and difficult to separate. The catalysts are loaded on inert carriers. After the reaction, the catalysts can be separated by simple filtration or centrifugation, but the catalytic efficiency of such catalysts will be greatly reduced. Therefore, the recovery and reuse of PPO catalyst is still a technical problem to be solved

Method used

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  • Supported catalyst and application thereof in preparing telechelic low-molecular-weight poly(phenylene oxide)
  • Supported catalyst and application thereof in preparing telechelic low-molecular-weight poly(phenylene oxide)
  • Supported catalyst and application thereof in preparing telechelic low-molecular-weight poly(phenylene oxide)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Preparation of Supported Catalysts

[0052] (1) Preparation of nano-alumina particles modified by silane coupling agent

[0053] Under mechanical stirring, 0.3mL (1.5mmol) of 3-mercaptopropyltrimethoxysilane and nano-alumina (1.9g) were refluxed at 110°C in a mixed solution of 100mL toluene / methanol=80:20 (volume ratio) for 24 Hour. After the reaction, the product was washed three times with methanol and three times with deionized water, centrifuged, and the separated solid was vacuum-dried for 48 hours to obtain nano-alumina particles modified by a silane coupling agent.

[0054] (2) Preparation of cross-linked polyvinylimidazole ligands grafted on the surface of nano-alumina particles

[0055] 2.72 mL (30 mmol) of N-vinylimidazole (30 mmol) distilled under reduced pressure, 0.42 mL (3 mmol) of divinylbenzene and 2 g of nano-alumina particles modified by the silane coupling agent prepared in step (1) were ultrasonically dispersed in 50 ml In ethyl acetate, adding N-...

Embodiment 2～4

[0060] Except for changing the feeding ratio of N-vinylimidazole and divinylbenzene, the rest of the operations are the same as in Example 1 to prepare the cross-linked polymer supported by nano-alumina particles. Cross-linked polymer ligand-metal ion complex catalyst.

[0061] Table 2

[0062] Example serial number N-vinylimidazole / divinylbenzene 2 2.72mL (30mmol) / 0.84mL (6mmol) 3 2.72mL (30mmol) / 1.40mL (10mmol) 4 2.72mL (30mmol) / 0.21mL (1.5mmol)

Embodiment 5～6

[0064] Except adopting 3-mercaptopropyltriethoxysilane and 4-mercaptobutyltrimethoxysilane to replace 3-mercaptopropyltrimethoxysilane in Example 1, all the other operations are the same as in Example 1 to prepare silane The nano-alumina particles modified by the coupling agent finally obtain the cross-linked polymer ligand-metal ion complex catalyst supported by the nano-alumina particles.

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Abstract

The invention discloses a supported catalyst which is a complex of metal ions and an imidazole ligand the surface of which is grafted with surface-modified nano-alumina particles. The surface-modifiednano-alumina particles are nano-alumina particles modified by a silane coupling agent. The catalyst has high catalytic efficiency and good selectivity, and can be separated from a reaction system bycentrifugation or filtration for recovery and recycling, solving the problem that current catalysts are difficult to recycle in the PPO production process. A product has the characteristics of a low residual metal catalyst content, a low dielectric constant, low dielectric loss, and good processing performance. Telechelic low-molecular-weight PPO can achieve cross-linking itself, can be chemicallymodified by reacting the terminal double bond with other substances, is simple and feasible in preparation process, has broad development space and great market application value, is suitable for industrial production, and meets the requirements of sustainable development.

Description

technical field [0001] The invention relates to the technical field of polymer chemical industry, in particular to a supported catalyst and a preparation method thereof, and the application of the supported catalyst in preparing telechelic low-molecular-weight polyphenylene ether in an oil-water two-phase medium. Background technique [0002] Polyphenylene oxide (PPO) is an engineering plastic with excellent comprehensive properties. It not only has good mechanical properties, but also has low dielectric constant, low dielectric loss, low moisture absorption, high glass transition temperature, acid and alkali corrosion resistance, etc. Outstanding performance, so it has broad application prospects in the fields of auto parts, electronic devices, office equipment, coatings and additives. However, as a thermoplastic resin, high molecular weight PPO has high melt viscosity, poor processability, and low reactivity when used in additives and composite materials. Low-molecular-we...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/44C08G65/48
CPCC08G65/44C08G65/485Y02P20/584
Inventor 黄家辉王奂张好磊郎绪志
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI