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A kind of synthetic method of polyphenylene ether

A synthesis method and polyphenylene ether technology are applied in the synthesis field of polyphenylene ether, which can solve the problem of high volatile content, achieve the effects of low volatility and saving methanol precipitant

Active Publication Date: 2020-07-28
INST OF CHEM ENG GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problem of excessive volatile matter content caused by the presence of organic amine / pyridine residues in copper amine / ammonium complexes or copper / pyridine complex catalysts in the prior art, the present invention provides a catalyst based on metal-guanidine complexation System Catalyzed Oxidative Coupling of Alkylphenols to Polyphenylene Ethers

Method used

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  • A kind of synthetic method of polyphenylene ether
  • A kind of synthetic method of polyphenylene ether
  • A kind of synthetic method of polyphenylene ether

Examples

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preparation example Construction

[0038] The synthetic method of this polyphenylene ether comprises the following steps:

[0039] 1) Catalyst preparation: dissolving cuprous salt and guanidine compound in a solvent, adding them into a reaction kettle for mixing and stirring, to obtain a catalyst;

[0040]2) Adding polymerized monomers: adding alkylphenol and solvent into the reaction kettle, mixing and stirring;

[0041] 3) Oxygen reaction: feed oxygen into the reactor to carry out polymerization reaction;

[0042] 4) Extracting the product: releasing the reaction solution in the reactor, concentrating, precipitating, and drying to obtain the polyphenylene ether product.

[0043] Preferably, the solvent described in step 1) or step 2) of the synthesis method is a benzene solvent; the temperature of the benzene solvent is 25° C. to 50° C.; further, the benzene solvent is toluene.

[0044] Preferably, in step 1) of the synthesis method, the volume of the reaction tank is 1L-3L.

[0045] Preferably, in step 1)...

Embodiment 1

[0058] Quickly weigh 1.15g of cuprous bromide and 0.70g of 1,3-dimethylguanidine at room temperature, dissolve them in 8mL of toluene, add them to the reaction kettle replaced by high-purity nitrogen for 2-3 times, and continue to add 488.48g of 2,6-dimethylphenol, wherein 2,6-dimethylphenol: cuprous bromide: 1,3-dimethylguanidine=100:0.2:0.2 (molar ratio). After adding an appropriate amount of toluene solvent until the total volume of the reaction solution reaches 1.8 L, start the stirring paddle and maintain the stirring speed at 200 r / min. After stirring for more than 10 minutes until the material is completely dissolved, the stirring rate is increased to 500r / min, and the pressure is 0.2bar. 50°C. After 1 h, the reaction was completed, and the material was released, concentrated and transferred to 10 L of methanol precipitant for precipitation to obtain a white flocculent solid. The collected precipitate was dried in a vacuum oven at 50°C for 6 hours, and then fully disp...

Embodiment 2

[0060] Quickly weigh 0.80g of cuprous chloride and 10.40g of polyhexamethylene biguanide hydrochloride (Mn=2600g / mol, PDI=1.18) at room temperature, dissolve them in 40mL of toluene, and add them to high-purity nitrogen replacement After 2 to 3 times, continue to add 488.48g of 2,6-dimethylphenol into the reactor, wherein 2,6-dimethylphenol: cuprous chloride: polyhexamethylene biguanide hydrochloride = 100: 0.2:0.1 (molar ratio). After adding an appropriate amount of toluene solvent until the total volume of the reaction solution reaches 1.8 L, start the stirring paddle and maintain the stirring rate at 150 r / min. After stirring for more than 10 minutes until the material is completely dissolved, the stirring rate is increased to 600r / min, and the pressure is 2 bar to start the reaction and release a large amount of heat. The chilled water is passed into the shell of the reactor to cool down, and the amount of chilled water is adjusted to maintain the reaction temperature at 2...

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Abstract

The invention discloses a synthesis method of polyphenylene ether. The synthesis method of the polyphenylene ether uses a metal-guanidine complex as a catalyst to synthesize polyphenylene ether through an oxidative coupling reaction of an alkyl phenol. The polyphenylene ether powder prepared by the present invention does not contain amine / ammonium, pyridine and other components, which solves the problem of organic amine / pyridine residues in the copper amine / ammonium complex or copper / pyridine complex catalyst, and avoids / reduces high temperature Production / residue of unpleasant odor during processing or processed products. The low-volatility polyphenylene ether powder prepared by the invention broadens the application scope of polyphenylene ether materials in fields such as earphone wires, data wires, and smart wearables that are sensitive to human body contact.

Description

technical field [0001] The invention relates to a synthesis method of polyphenylene ether. Background technique [0002] Polyphenylene oxide (PPO) is one of the five general-purpose engineering plastics in the world. It has the advantages of high strength, high temperature resistance, non-toxicity, halogen-free flame retardant, low density, and low dielectric loss. Polyphenylene ether is a non-crystalline resin with no hydrophilic group in its molecular structure. It has excellent hydrolysis resistance, low moisture absorption rate, good dimensional stability, and low creep value under high load strength. There are no highly polar groups in the molecular structure of polyphenylene ether, no dipole polarization, and a symmetrical structure, so it has excellent dielectric properties and can maintain good dielectric properties in a wide range of temperature, humidity and frequency . Its dielectric constant and dielectric loss tangent are the smallest, ranking first among engi...

Claims

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Application Information

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IPC IPC(8): C08G65/44
CPCC08G65/44
Inventor 李伟浩彭小权麦裕良钟本镔江川霞许可
Owner INST OF CHEM ENG GUANGDONG ACAD OF SCI
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