Method for preparing polyphenyl ether with side chain containing unsaturated carbon-carbon double bond in water medium

An unsaturated and carbon double bond technology is applied in the field of preparing polyphenylene ethers containing unsaturated carbon-carbon double bonds in the side chain, and can solve the problems of high catalyst metal ion content, high glass transition temperature, large molecular weight of PPO, etc. Achieve the effect of large market application value, low dielectric constant and low metal ion content

Inactive Publication Date: 2013-06-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention finds: if can use the phenolic monomer containing unsaturated carbon-carbon double bond to carry out copolymerization reaction with conventional phenolic monomer in aqueous medium, then can simultaneously solve existing in the prior art " synthesis in organic solvent The PPO molecular weight is large, its glass transition temperature is high and it is not easy to process, and due to the homogeneous reaction, the residual catalyst metal ion content in the product is relatively high, which reduces its electrical properties to a certain extent. Introducing unsaturated carbon-carbon double bonds into PPO to modify polyphenylene ether and expand its scope of use”, and the molecular weight of PPO synthesized in aqueous medium is small, which is easy to process

Method used

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  • Method for preparing polyphenyl ether with side chain containing unsaturated carbon-carbon double bond in water medium
  • Method for preparing polyphenyl ether with side chain containing unsaturated carbon-carbon double bond in water medium
  • Method for preparing polyphenyl ether with side chain containing unsaturated carbon-carbon double bond in water medium

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Example 1 Preparation of Polyphenylene Ether with Side Chain Containing Unsaturated Carbon-Carbon Double Bonds in Aqueous Medium

[0044] In a reaction kettle with a stirring paddle and a thermometer, add sodium hydroxide (0.2g, 5mmol), sodium lauryl sulfate (0.1694g, 0.5mmol), 2,6-dimethylphenol (DMP, 0.4930g , 4mmol), 2-allyl-6-methylphenol (AMP, 0.15ml, 1mmol) and distilled water 100mL, after stirring evenly, raise the temperature of the reactor to 50℃, then add copper chloride (0.0086g, 0.05 mmol) / ethylenediaminetetraacetic acid (EDTA, 0.05mmol) complex, fed with oxygen, and reacted for 24 hours at a stirring speed of 600rotor / min (rev / min). After the reaction, add sodium chloride to break the emulsion, then filter, wash with water, and vacuum-dry to constant weight to obtain a solid product, that is, polyphenylene ether containing double bonds, with a yield of 78.35%, a weight average molecular weight of 6000, and a molecular weight distribution of 2.2, m= 17, n=4...

Embodiment 2～3

[0046] According to the method of Example 1, polyphenylene ether containing unsaturated carbon-carbon double bonds in the side chain was prepared in the aqueous medium, the difference was that the ratio of the two phenolic monomers was changed. The polymerization results are shown in Table 1:

[0047] Table 1

[0048]

Embodiment 4

[0050] According to the method of Example 1, polyphenylene ether containing unsaturated carbon-carbon double bonds in the side chain was prepared in aqueous medium, except that 0.52 g (5.2 mmol) of potassium bicarbonate was used instead of sodium hydroxide, and the yield was 76.57%. The product The weight average molecular weight is 5900, the molecular weight distribution is 2.1, m=18, n=4, and the residual copper ion content is 0.76ppm.

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Abstract

The invention discloses a method for preparing polyphenyl ether with a side chain containing an unsaturated carbon-carbon double bond in a water medium. The method comprises the following steps of: carrying out oxidative copolymerization reaction on a common phenol monomer and a phenol monomer containing the unsaturated carbon-carbon double bond in the water medium at 30-60 DEG C for 4-24 hours in the presence of a catalyst, a surfactant, an alkali compound and an oxidant; and after the oxidative copolymerization reaction is finished, carrying out demulsification, filtering and washing to obtain the polyphenyl ether with the side chain containing the unsaturated carbon-carbon double bond. The polyphenyl ether containing the unsaturated carbon-carbon double bond prepared in the water medium according to the method disclosed by the invention has the characteristics of low residual metal catalyst content, low dielectric constant, low medium loss, organic solvent resistance, high temperature resistance, good processing performance and the like; and the preparation process is green, environment-friendly, simple, convenient, and easy to implement, safe and nontoxic, has wide development space and great market application value, and is 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 method for preparing polyphenylene ether with side chains containing unsaturated carbon-carbon double bonds in an aqueous medium. Background technique [0002] Poly 2,6-dimethylphenylene oxide (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, high glass transition temperature, Outstanding properties such as acid and alkali corrosion resistance, especially excellent electrical properties (ε=2.5-2.6, tanδ=0.0015-0.0019). However, PPO is a kind of thermoplastic resin, which cannot withstand the requirements of welding at high temperature, and is easily soluble in aromatic hydrocarbons or chlorinated aliphatic hydrocarbons. It has poor solvent resistance and poor film-forming properties. Therefore, polyphenylene ether must be modified to ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/44
Inventor 王奂申屠宝卿翁志学
Owner ZHEJIANG UNIV
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