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A supported catalyst and its application in the preparation of cross-linkable polyphenylene ether

A technology of supported catalyst and polyphenylene ether, which is applied in the field of supported catalyst and its preparation, and the preparation of crosslinkable polyphenylene ether, which can solve the problems of difficult separation and reduced catalytic efficiency, and achieve easy control, simple operation, The effect of large market application value

Active Publication Date: 2022-07-08
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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  • A supported catalyst and its application in the preparation of cross-linkable polyphenylene ether
  • A supported catalyst and its application in the preparation of cross-linkable polyphenylene ether
  • A supported catalyst and its application in the preparation of cross-linkable polyphenylene ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Preparation of supported catalysts

[0048] (1) Preparation of Nano-Alumina Particles Modified by Silane Coupling Agent

[0049] Under mechanical stirring, 0.3 mL (1.5 mmol) of 3-mercaptopropyltrimethoxysilane and nano-alumina (1.9 g) in a mixed solution of 100 mL of toluene / methanol=8:2 (volume ratio) were reacted at 110°C under reflux for 24 Hour. After the reaction, the product was washed 3 times with methanol, 3 times with deionized water, centrifuged, and the separated solid was vacuum-dried for 48 hours to obtain nano-alumina particles modified with a silane coupling agent.

[0050] (2) Preparation of cross-linked polyvinylimidazole ligands grafted on the surface of nano-alumina particles

[0051] 2.72 mL (30 mmol) of N-vinylimidazole distilled under reduced pressure, 0.42 mL (3 mmol) of divinylbenzene, and 2 g of the silane coupling agent-modified nano-alumina particles prepared in step (1) were ultrasonically dispersed in 50 mL. In ethyl acetate, azobisisobut...

Embodiment 2～4

[0056] Except changing the feeding ratio of N-vinylimidazole and divinylbenzene, other 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 catalysts.

[0057] Table 2

[0058] 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

[0060] Except that 3-mercaptopropyltriethoxysilane and 4-mercaptobutyltrimethoxysilane were used instead of 3-mercaptopropyltrimethoxysilane in Example 1, other operations were the same as those in Example 1. The nano-alumina particles modified by the linking agent are finally obtained as a 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 and its application in preparing cross-linkable polyphenylene ether, which is a complex of imidazole ligands and metal ions grafted on the surface of surface-modified nano-alumina particles; The surface-modified nano-alumina particles are nano-alumina particles modified by a silane coupling agent. The catalyst of the invention has high catalytic efficiency and good selectivity, and can be separated from the reaction system by means of centrifugation or filtration, recovered and recycled. The problem that the current catalyst is difficult to recycle in the PPO production process is solved. The product has the characteristics of less residual metal catalyst content, low dielectric constant and dielectric loss, resistance to organic solvents after cross-linking and curing, high temperature resistance, good processing performance, etc. The preparation process is simple and easy, and has broad development space and great market application. Value, suitable for industrial production, in line with 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, as well as the application of the supported catalyst in preparing cross-linkable polyphenylene ether in an oil-water two-phase medium. Background technique [0002] Polyphenylene ether (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 hygroscopicity, high glass transition temperature, acid and alkali corrosion resistance, etc. Outstanding performance, but as a thermoplastic resin, PPO cannot withstand the requirements of high temperature welding, and is easily soluble in aromatic hydrocarbons or chlorinated aliphatic hydrocarbons, and has poor solvent resistance. The introduction of unsaturated carbon-carbon double bonds into PPO is a good solution to the above-mentioned problems....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/44
CPCC08G65/44C08G2650/56Y02P20/584
Inventor 黄家辉王奂陈锴王晓光
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI