Polyfunctional group polyphenylene ether resin and preparation method thereof

A polyphenylene ether resin and multifunctional technology, which is applied in the field of preparation of organic polymer compounds, can solve the problems of increasing the difficulty of the reaction process, the complexity of the equipment and the manufacturing cost, and achieve the effect of excellent performance, good performance and good fluidity

Active Publication Date: 2014-12-24
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] EP1489079A1 mentioned the method of anhydride capping of polyphenylene ether molecules, using low-molecular-weight bifunctional polyphenylene ether to react with trimellitic anhydride acid chloride, because the acid chloride is easily hydrolyzed, which increases the difficulty of the reaction process and the complexity of equipment and manufacturing costs
[0006] In summary, the existing technology still has great limitations in the modification of polyphenylene ether

Method used

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  • Polyfunctional group polyphenylene ether resin and preparation method thereof
  • Polyfunctional group polyphenylene ether resin and preparation method thereof
  • Polyfunctional group polyphenylene ether resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]First, add 100 kg of polyphenylene ether (Asahi Kasei Chemical Co., Ltd., trade name S201A, number average molecular weight is 20000) in a non-airtight reactor A equipped with a reflux condenser, stirring, and a thermocouple, and add 210 kg of toluene As a solvent, heat up to 90°C and stir to dissolve the polyphenylene ether completely, then add 15.4kg of diallyl bisphenol A, at 90°C, add 4kg of benzoyl peroxide, add 6 times in half an hour , Stop the reaction after 3h. Second, add 2.2kg of sodium hydroxide and 1kg of tetrabutylammonium bromide to reactor A, add 30.4kg of 3-chloropropene dropwise at a temperature of 50°C, drop it for 1 hour, and continue the reaction at this temperature After 8 hours, the reaction solution of allylated polyphenylene ether resin was obtained. Thirdly, the allylated polyphenylene ether resin reaction solution obtained in reactor A was distilled, and the fraction at 50° C. was recovered. After there was no distillate, 18 kg of peroxyaceti...

Embodiment 2

[0039] First, add 100kg of polyphenylene ether (Blue Star New Materials, trade name LXR35, number average molecular weight 22000-28000) into a non-airtight reactor A equipped with a reflux condenser, stirring and thermocouple, and add 300 Use ㎏ toluene as a solvent, heat up to 84°C and stir to dissolve polyphenylene ether completely, then add 19㎏ tetraallyl bisphenol A, at 90°C, add 4 kg of benzoyl peroxide at one time, and react for 4 hours Stop responding. Second, add 2.2kg of sodium hydroxide and 2kg of tetrabutylammonium bromide to reactor A, add 19.4kg of 3-chloropropene dropwise at a temperature of 40°C, drop it in 0.75h, and continue at this temperature After reacting for 6 hours, an allylated polyphenylene ether resin reaction solution was obtained. Thirdly, distill the allylated polyphenylene ether resin reaction solution obtained in reactor A, and recover the fraction at 60°C. After there is no distillate, add 18 kg of peroxyacetic acid (40% content) and react at 4...

Embodiment 3

[0042] First, add 100 kg of polyphenylene ether (Asahi Kasei Chemical Co., Ltd., trade name S201A, number average molecular weight is 20000) in a non-airtight reactor A equipped with a reflux condenser, stirring, and a thermocouple, and add 210 kg of two Use toluene as solvent, heat up to 90°C and stir to dissolve polyphenylene ether completely, then add 15.4kg of diallyl bisphenol A, at 84°C, add 2.7kg of di-tert-butyl peroxide, three times in half an hour After the addition was completed, the reaction was stopped after 5 hours of reaction. Second, add 0.7kg of sodium hydroxide and 1.4kg of tetrabutylammonium chloride to reactor A, add 12.4kg of 3-chloropropene dropwise at a temperature of 30°C, drop it for 1 hour, and continue the reaction at this temperature After 8 hours, the reaction solution of allylated polyphenylene ether resin was obtained. Thirdly, the allylated polyphenylene ether resin reaction solution obtained in reactor A was distilled, and the fraction at 50° ...

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Abstract

The invention discloses polyfunctional group polyphenylene ether resin and a preparation method thereof. The method is characterized by comprising the following steps: in a reactor, adding polyphenyl ether, a solvent and diallyl bisphenol A or tetraallyl bisphenol A, and adding a peroxide initiator for reaction for 1-10h at 30-90 DEG C; adding alkali metal hydroxides and a phase transfer catalyst, and dropwise adding 3-allyl chloride for reaction for 6-24h at 30-50 DEG C; distilling a reaction solution, recovering fraction below 50 DEG C, and then adding 40% peracetic acid for reaction for 5-15h at 20-60 DEG C; extracting the reaction solution with deionized water for three times, distilling off most of the solvent from the extraction liquid, then dropwise adding the residual solution in methanol for precipitation and filtration, and finally washing solids with methanol and drying to obtain the polyfunctional group polyphenylene ether resin. The polyphenylene ether resin and other resins can form a composition with multiple uses, and the polyphenylene ether resin can be used for manufacturing films or copper coated substrates of printed circuit boards and other fiber cloth laminated boards.

Description

technical field [0001] The invention belongs to the preparation of organic macromolecular compounds, and relates to a preparation method of polyphenylene ether resin with multifunctional groups (containing epoxy groups, hydroxyl groups and double bonds). The multifunctional polyphenylene ether resin prepared by the invention can form different multi-purpose compositions with other resins, and is used for making films of printed circuit boards or copper-clad substrates and other fiber cloth laminates. Background technique [0002] With the rapid development of the information industry, higher requirements have been put forward 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 (PPE) has good comprehensive properties, especially high glass transition temperature and excellent dielectric properties, and is on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C08L71/12
Inventor 代三威黄杰吴学明
Owner SICHUAN DONGFANG INSULATING MATERIAL
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