Synthesis method of double-end hydroxy polyphenylene ether oligomer

A double-ended hydroxyl polyphenylene ether, synthesis method technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, chemical/physical processes, etc., can solve the problem of low reactivity, residual polyphenol monopoly In order to improve product quality, improve product hydroxyl content, and promote the effect of reaction

Active Publication Date: 2019-03-26
GUANGDONG RES INSTITITUTE OF PETROCHEM & FINE CHEM ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to overcome the defect of prior art, provide a kind of synthetic method of double-terminated hydroxyl polyphenylene ether oligomer, solve the low reactivity between primary phenol and polyphenol in conventional catalytic system, residual polyphenol monomer is comparatively low many questions

Method used

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  • Synthesis method of double-end hydroxy polyphenylene ether oligomer
  • Synthesis method of double-end hydroxy polyphenylene ether oligomer
  • Synthesis method of double-end hydroxy polyphenylene ether oligomer

Examples

Experimental program
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Effect test

Embodiment 1

[0052] A kind of synthetic method of double-terminated hydroxyl polyphenylene ether oligomer, comprises the following steps:

[0053] 1) Add 335.50g of 2,6-dimethylphenol, 57.00g of bisphenol A, 779.13g of toluene and 114.00g of methanol into a reaction kettle with a condensation reflux device, stir until the monomers are completely dissolved, then add 16.50g of ten Dialkylpolyethyleneimine ligands (M n =2000) and 6.17g cuprous bromide hydrobromic acid solution (freshly prepared with 0.45g cuprous oxide and 5.72g 48% hydrobromic acid in advance), mix well, feed oxygen (flow rate is 200sccm), 40 ℃ of reaction 150min;

[0054] 2) Add the reacted polymer solution into 50.81mL of 10% trisodium nitrilotriacetate solution, react at 70°C for 60min, and remove the aqueous phase by liquid-liquid centrifugation;

[0055] 3) Concentrate the oil phase obtained by centrifugation in step 2) to about 900mL, then add 9000mL of methanol to precipitate, filter, wash with methanol for 3 times,...

Embodiment 2

[0057] A kind of synthetic method of double-terminated hydroxyl polyphenylene ether oligomer, comprises the following steps:

[0058] 1) Add 305.00g of 2,6-dimethylphenol, 47.33g of tetramethylbisphenol A, 942.62g of toluene and 94.00g of methanol into a reaction kettle with a condensation reflux device, stir until the monomers are completely dissolved, then add 12.53g branched polyethyleneimine ligand (M n =600) and 4.11g cuprous bromide hydrobromic acid solution (freshly prepared with 0.30g cuprous oxide and 3.81g 48% hydrobromic acid in advance), mix well, pass into oxygen (flow rate is 200sccm), 40 ℃ of reaction 150min;

[0059] 2) Add the reacted polymer solution into 33.87mL 10% trisodium nitrilotriacetate solution, react at 70°C for 60min, and remove the water phase by liquid-liquid centrifugation;

[0060] 3) Concentrate the oil phase obtained by centrifugation in step 2) to about 900mL, then add 9000mL of methanol to precipitate, filter, wash with methanol for 3 tim...

Embodiment 3

[0062] A kind of synthetic method of double-terminated hydroxyl polyphenylene ether oligomer, comprises the following steps:

[0063] 1) Add 341.60g of 2,6-dimethylphenol, 80.00g of bisphenol F, 801.26g of toluene and 160.00g of methanol into a reaction kettle with a condensing reflux device, stir until the monomers are completely dissolved, then add 16.85g of linear Polyethyleneimine ligand (M n =1200) and 5.22g cuprous chloride hydrochloric acid solution (freshly prepared with 0.60g cuprous oxide and 4.62g 37% hydrochloric acid in advance), mix uniformly, pass into oxygen (flow rate is 200sccm), 45 ℃ of reaction 150min;

[0064] 2) Add the reacted polymer solution into 33.87mL 20% trisodium nitrilotriacetate solution, react at 70°C for 60min, and remove the aqueous phase by liquid-liquid centrifugation;

[0065] 3) Concentrate the oil phase obtained by centrifugation in step 2) to about 900mL, then add 9000mL of methanol to precipitate, filter, wash with methanol for 3 time...

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Abstract

The invention discloses a synthesis method of a double-end hydroxy polyphenylene ether oligomer. In the synthesis method of the double-end hydroxy polyphenylene ether oligomer, the double-end hydroxypolyphenylene ether oligomer is obtained by taking a metal-polyethyleneimine complex as a catalyst through an oxidative copolymerization reaction of monohydric phenol and dihydric phenol. According tothe synthesis method, the metal-polyethyleneimine complex is used as the catalyst, the catalytic activity is milder, the reaction between the dihydric phenol and the monohydric phenol can be effectively promoted, the hydroxyl content of the product is increased, and the residue of the dihydric phenol monomer of the product is simultaneously reduced and the product quality is improved. The double-end hydroxy polyphenylene ether oligomer prepared by the invention can be used as an additive and a copolymerization block of other thermoplastics, thermoplastic elastomers and thermosetting materialsto improve the thermal property, adhesive force, mechanical property and chemical resistance and electrical property of the material.

Description

technical field [0001] The invention relates to a method for synthesizing double-terminated hydroxyl polyphenylene ether oligomers. Background technique [0002] The rapid development of the information industry has put forward higher requirements for the matrix resin for copper clad laminates, requiring it to have low dielectric constant and dielectric loss, high glass transition temperature, high heat resistance, and low water absorption. Polyphenylene ether resin (PPO) is one of the five general-purpose engineering plastics in the world. Its molecular structure is a highly rigid skeleton chain of aromatic rings, and has no strong polar groups. It has good heat resistance, flame retardancy, low hygroscopicity and Dimensional stability, especially excellent dielectric properties in a wide temperature range, is one of the ideal substitute materials for high-performance copper clad laminate substrates. [0003] However, conventional polyphenylene ether resins have high melt ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/44
CPCC08G65/44C08G65/46B01J31/1683B01J31/1805B01J2531/16B01J2531/72B01J2531/845B01J2531/842B01J31/12
Inventor 麦裕良钟本镔李伟浩彭小权许可
Owner GUANGDONG RES INSTITITUTE OF PETROCHEM & FINE CHEM ENG
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