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Alkynyl-terminated polyphenyl ether as well as preparation method and application thereof

A polyphenylene ether and alkynyl technology, which is applied in the field of alkynyl-terminated polyphenylene ether compounds and their preparation, can solve the problem that it is difficult to ensure that the end-capped group does not undergo a curing reaction in advance, and the cross-linking density of double bonds and other resins Limited, low efficiency of end-capped polyphenylene ether, etc., to achieve the effect of excellent processability, low intrinsic viscosity, and reduction of process steps

Pending Publication Date: 2022-02-25
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, polyphenylene ether is mostly used for capping reaction with compounds containing carbon-carbon double bonds such as unsaturated halogenated hydrocarbons and acid anhydrides, and carbon-carbon double bond groups that can be cross-linked and cured are introduced into polyphenylene ether. , the heat resistance of the prepared composite material is improved, but the crosslinking density of the double bond and other resins is limited; CN110437439A discloses a synthesis method of alkenyl-terminated polyphenylene ether, which is washed by alkaline aqueous solution and phenolic monomer The double-terminal hydroxyl polyphenylene ether solution obtained by the oxidative copolymerization reaction, and then the oil phase product obtained by separation is subjected to a capping reaction with an alkenyl reagent. This method reduces the traditional treatment process of purifying the polyphenylene ether solution, but prepares the capped polyphenylene ether solution. The efficiency of ether is still not high; CN101921394A discloses a method for capping polyphenylene ether by other groups such as double bonds, by drying the wet powder of polyphenylene ether, and using a capping compound to carry out capping reaction on polyphenylene ether , the operation process is complicated, and it is difficult to ensure that the end-capping group does not undergo curing reaction in advance during the high-temperature drying process, which will have an adverse effect on product performance

Method used

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  • Alkynyl-terminated polyphenyl ether as well as preparation method and application thereof
  • Alkynyl-terminated polyphenyl ether as well as preparation method and application thereof
  • Alkynyl-terminated polyphenyl ether as well as preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0030] Put 0.31g of cuprous chloride, 25ml of pyridine, and 50ml of toluene into a 250ml four-neck flask, start mechanical stirring, and maintain the system temperature at 30°C under the protection of oxygen, and it can be observed that the color of the solution turns dark green immediately. In addition, prepare a mixture of 20.18g of 2,6-dimethylphenol, 4.75g of 2,2-bis(4-hydroxy-3,5-dimethylphenyl)propane and 75ml of toluene, and slowly pour it into the above-mentioned four-necked bottle. The mixed solution was added dropwise, and the solution immediately turned yellow-brown. After 2 hours of dropwise addition, the reaction was completed for 4 hours. As the reaction progressed, a pale yellow powder precipitated out. The reaction liquid is poured into 5% hydrochloric acid-methanol solution, and the resin is precipitated, washed with methanol and water, filtered, and dried to obtain a low molecular weight polyphenylene ether. The calculated yield of the low-molecular-weight po...

Embodiment 2

[0033] Put 0.2g of cuprous chloride, 16ml of pyridine, and 40ml of methanol into a 250ml four-neck flask, keep the temperature of the system at 30°C, feed oxygen, start mechanical stirring, and the color of the solution turns dark green immediately. In addition, prepare a mixture of 19.52g of 2,6-dimethylphenol, 4.55g of 2,2-bis(4-hydroxy-3,5-dimethylphenyl)propane and 60ml of methanol, and slowly pour it into the above-mentioned four-necked bottle. The mixed solution was added dropwise, and the solution immediately turned yellow-brown, and the dropwise addition was completed in 2 hours. As the reaction progressed, a pale yellow powder precipitated out, and the reaction was completed in 4 hours. The reaction liquid is directly suction-filtered, and the filter cake is the product, which is then washed with methanol and water, and dried on a heating plate at 120°C to constant weight to obtain low-molecular-weight polyphenylene ether. The calculated yield of the low-molecular-wei...

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Abstract

The invention discloses alkynyl-terminated polyphenyl ether as well as a preparation method and application thereof. The structural formula of the alkynyl-terminated polyphenyl ether is shown in the specification. Low-molecular-weight polyphenyl ether and propargyl bromide are subjected to a termination reaction under an alkaline condition, and separation and purification are performed to obtain the alkynyl-terminated polyphenyl ether. The preparation method has the characteristics of simplicity in operation, low cost and high yield. By reacting propargyl bromide with low-molecular-weight polyphenyl ether, a carbon-carbon triple bond group which is relatively high in activity and can be cross-linked and cured at a certain temperature is introduced into polyphenyl ether, so that the polyphenyl ether has excellent dielectric property and relatively low intrinsic viscosity. Through crosslinking curing of alkynyl or with other resins, the mechanical strength, solvent resistance, heat resistance, flame retardance and the like of the cured material are improved, and application of the material in a high-performance copper-clad plate is facilitated.

Description

technical field [0001] The invention belongs to the field of polyphenylene ether modification, and in particular relates to an alkynyl-terminated polyphenylene ether compound and a preparation method and application thereof. Background technique [0002] With the rapid development of electronic information, printed circuit boards have become the main components of most electronic products, so the substrate copper clad laminate (CCL) as a printed circuit board has also been vigorously developed, and the matrix resin material is the key material of CCL One of them determines the mechanical strength, processing performance, heat resistance, and dielectric properties of the printed circuit board. Polyphenylene ether resin (PPO) is one of the five major engineering plastics, with good mechanical properties, heat resistance and dimensional stability, especially polyphenylene ether has low dielectric properties in a wide temperature and frequency range Loss, so it is an ideal mate...

Claims

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Application Information

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IPC IPC(8): C08G65/48C08L71/12C08J5/18
CPCC08G65/485C08J5/18C08J2371/12
Inventor 刘锋冯英敏
Owner ZHENGZHOU UNIV
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