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Low-molecular-weight functionalized star-shaped polyphenyl ether and preparation method thereof

A technology of functionalized molecular weight and low molecular weight, which is applied in the field of low molecular weight functionalized star polyphenylene ether and its preparation, can solve the problems of high functional group content, low reactive functional group, difficult processing of polyphenylene ether, etc., and achieve good mechanical properties and medium The effect of low electrical constant and excellent product performance

Active Publication Date: 2021-11-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the shortcomings of polyphenylene ether in the prior art, such as difficult processing, poor solubility, and low reactive functional groups, and provide a method for redistribution and terminal functionalization of low-molecular-weight functionalized star-shaped polyphenylene ether. Products with low molecular weight, high functional group content, excellent solubility, reactivity, thermosetting, compatibility and dielectric properties

Method used

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  • Low-molecular-weight functionalized star-shaped polyphenyl ether and preparation method thereof
  • Low-molecular-weight functionalized star-shaped polyphenyl ether and preparation method thereof
  • Low-molecular-weight functionalized star-shaped polyphenyl ether and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1 Manufacture and performance test of low molecular weight polyhydroxylated star polyphenylene ether (TH-1)

[0062] Mix 100.0g polyphenylene ether raw material (molecular weight 23560), 20.0g 1,1,1-tris(4-hydroxyphenyl)propane, add to a three-neck round bottom flask equipped with a thermometer and a stirrer, add 700g toluene As a solvent, raise the temperature to 85°C and stir thoroughly for 30 minutes, then dissolve 8.0 g of benzoyl peroxide in a mixed solvent consisting of 75 g of toluene and 25 g of methanol, and add it to the reaction system evenly within 3 hours, and continue stirring after the addition is complete 5h.

[0063] After the reaction was completed, methanol with a mass fraction of 25% was added to the reaction liquid, and the mixture was fully stirred for 30 minutes, and the precipitated macromolecular polyphenylene ether residue was filtered. Then use 10% aqueous sodium bicarbonate solution and deionized water to wash the remaining reacti...

Embodiment 2

[0067] Embodiment 2 Manufacture and performance test of low molecular weight polyhydroxylated star polyphenylene ether (TH-2)

[0068] Mix 100.0g polyphenylene ether raw material (molecular weight: 23560), 10.0g 1,1,1-tris(4-hydroxyphenyl)propane, add to a three-necked round bottom flask equipped with a thermometer and stirrer, add 700g toluene As a solvent, raise the temperature to 85°C and stir thoroughly for 30 minutes, then dissolve 3.0 g of benzoyl peroxide in a mixed solvent composed of 75 g of toluene and 25 g of methanol, and add it to the reaction system evenly within 3 hours, and continue stirring after the addition is complete 5h.

[0069] After the reaction was completed, methanol with a mass fraction of 25% was added to the reaction liquid, and the mixture was fully stirred for 30 minutes, and the precipitated macromolecular polyphenylene ether residue was filtered. Then the remaining reaction solution was poured into 5000 g of methanol to precipitate a solid, an...

Embodiment 3

[0076] Example 3 Manufacture and Performance Test of Low Molecular Weight Acrylated Star Polyphenylene Ether

[0077] Take 20.0g TH-1 and dissolve it in a three-necked flask containing 100g toluene, install a serpentine condenser, a thermometer and a stirrer, add 8.0g methacrylic anhydride, add 0.2g N,N-dimethylaminopyridine, Raise the temperature to 85°C and start the reaction under stirring. After 5 hours, add the reaction solution into 1000g of methanol solution to precipitate a solid, and filter to obtain a low molecular weight propylene-based star polyphenylene ether, which is designated as THV-1. The product yield It was 94%, and the product molecular weight obtained by GPC method was 2306, and the molecular weight distribution index was 1.73. Proton nuclear magnetic resonance spectrum and infrared spectrum can show that it has a star structure with terminal propenyl groups, and its infrared spectrum is as follows image 3 As shown,.

[0078] Dissolve 10.0g THV-1 in ...

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Abstract

The invention relates to the technical field of polymer synthesis, and discloses low-molecular-weight functionalized star-shaped polyphenyl ether and a preparation method thereof. The preparation method comprises the following steps of 1, subjecting polyphenyl ether, a polyphenol hydroxyl compound and an initiator to a redistribution reaction in a solvent, then conducting a grading procedure to obtain a solution I, and carrying out post-treatment to obtain the low-molecular-weight polyhydroxylated star-shaped polyphenyl ether; and 2, dissolving the low-molecular-weight polyhydroxylated star-shaped polyphenyl ether, carrying out a functionalization end-capping reaction with a functionalization reagent to obtain a solution II, and carrying out post-treatment to obtain the low-molecular-weight functionalized star-shaped polyphenyl ether. By introducing the polyphenol hydroxyl compound, the functionalized star-shaped polyphenyl ether with the molecular weight of 4000 or less is obtained, and the polyphenyl ether can be directly cured to be used as an electronic material and is low in dielectric constant, good in mechanical property and excellent in effect.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a low molecular weight functionalized star polyphenylene ether and a preparation method thereof. Background technique [0002] The rapid development of communication technology has put forward new requirements for electrical components, that is, while maintaining appropriate thermodynamic properties, they have the ability to transmit information at high frequencies and high speeds. Taking printed circuit boards as an example, traditional PCB boards are mainly made of FR-4 boards made of epoxy resin with excellent cost performance, but this material cannot meet the requirements due to its insufficient electrical properties (dielectric constant Dk>4). Demand for high frequency and high speed products. From the perspective of preventing loss in signal transmission, it is necessary to introduce materials with low dielectric constant and low dielectric loss tangent into ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C08L63/00C08L71/12
CPCC08G65/485C08L63/00C08L71/126
Inventor 张才亮闫沁宇顾雪萍冯连芳
Owner ZHEJIANG UNIV
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