Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for modifying dihydroxy-terminated polyphenyl ether

A technology of double-terminated hydroxyl polyphenylene ether and polyphenylene ether, which is applied in the field of polyphenylene ether modification, can solve the problems of low utilization rate of reactants, high cost of anhydride route, and difficulty in removing halogens, so as to improve electrophilic ability and avoid Halogen residues and the effect of simplifying the production process

Active Publication Date: 2022-01-21
QINGDAO SANLI BENNUO CHEM IND +1
View PDF5 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the acid chloride route has the disadvantages of difficult halogen removal and complicated process; the acid anhydride route has the disadvantages of high cost and low utilization rate of reactants; the methacrylic acid route has the disadvantages of low reactant utilization rate and low end group modification rate

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for modifying dihydroxy-terminated polyphenyl ether
  • Method for modifying dihydroxy-terminated polyphenyl ether
  • Method for modifying dihydroxy-terminated polyphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0043] In the present invention, the preparation method of the double-terminated hydroxyl polyphenylene ether preferably includes the following steps:

[0044] Mix 2,6-dimethylphenol, dihydric phenol, organic solvent, catalyst and oxidant, and react at 20-70°C for 4-20 hours to obtain a polymerization liquid;

[0045] The polymerization solution and the chelating agent are mixed for chelation to obtain double-terminated hydroxyl polyphenylene ether;

[0046] The catalyst is an aqueous solution containing metal and amine ligands.

[0047] In the present invention, it is preferred to mix 2,6-dimethylphenol, dihydric phenol, organic solvent, catalyst and oxidant, and react at 20-70° C. for 4-20 hours to obtain a polymerization liquid. In the present invention, the molar ratio of 2,6-dimethylphenol to dihydric phenol is preferably 1˜15:1, more preferably 9:1. In the present invention, the dihydric phenol is preferably shown in structure (II):

[0048]

[0049] where R 1 , R...

Embodiment 1

[0058] (1) Add 0.598 kg of cuprous chloride and 0.702 kg of hexamethylenediamine to the catalyst preparation kettle, and add 0.6 kg of distilled water. After mixing evenly, stir for 1 hour under anaerobic conditions to obtain the catalyst. Add 53.5kg of 2,6-xylenol, 14kg of tetramethylbisphenol A and 250kg of toluene organic solvent in sequence, stir until the phenolic monomers are completely dissolved; then add the catalyst prepared above, then pass in oxygen, and react at 40°C 6h;

[0059] (2) After the reaction, add 35L 5%wt ethylenediaminetetraacetic acid disodium salt aqueous solution into the reaction kettle, stir at 70°C for 1h, then let it stand for 5h, remove the water phase, and obtain the double-terminated hydroxyl polyphenylene ether oligomer solution;

[0060] (3) After adding 260g DMAP (4-dimethylaminopyridine) to the solution of double-terminated hydroxyl polyphenylene ether oligomer obtained in step (2) and mixing evenly, after dissolving 3.01kg DCC (dicyclohe...

Embodiment 2

[0064] (1) Add 0.543kg of cuprous bromide and 0.757kg of dodecyl diamine to the catalyst preparation kettle, and add 0.7kg of distilled water, after mixing evenly, stir for 1 hour under anaerobic conditions to obtain the catalyst; Add 53.5kg of 2,6 dimethylphenol, 12.38kg of tetramethylbisphenol F and 238kg of toluene organic solvent, stir until the phenolic monomers are completely dissolved; then add the above catalyst, then pass in oxygen, and react at 40°C for 6 hours;

[0065] (2) After the reaction, add 70L 5%wt ethylenediaminetetraacetic acid disodium salt aqueous solution into the reaction kettle, stir at 50°C for 1h, then let it stand for 3h, remove the water phase, and obtain the double-terminated hydroxyl polyphenylene ether oligomer solution;

[0066] (3) Add 260g of DMAP to the purified double-terminated hydroxyl polyphenylene ether oligomer solution obtained in step (2) and mix evenly, then dissolve 3.01kg of DCC and drop it into the reactor, and add 10.46kg of me...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a method for modifying dihydroxy-terminated polyphenyl ether, and belongs to the technical field of polyphenyl ether modification. The method for modifying the double-terminal hydroxyl polyphenyl ether comprises the following steps: mixing the double-terminal hydroxyl polyphenyl ether, 4-dimethylaminopyridine and dicyclohexylcarbodiimide, and reacting for 50 to 70 minutes at the temperature of 20 to 100 DEG C so as to obtain a first reactant; mixing methacrylic acid with 4-dimethylaminopyridine, and carrying out a reaction at 20-100 DEG C for 50-70 min to obtain a second reactant; and mixing the first reactant and the second reactant, and reacting at 20-100 DEG C for 5.5-6.5 hours to obtain the modified polyphenyl ether solution. According to the method, methacrylic acid is used for end group modification, the halogen removal step can be omitted, halogen residues are avoided, the production process is simplified, the efficiency is improved, the utilization rate of methacrylic acid is high, and the cost can be further reduced.

Description

technical field [0001] The invention belongs to the technical field of polyphenylene ether modification, and in particular relates to a method for modifying double-terminated hydroxyl polyphenylene ether. Background technique [0002] Polyphenylene oxide (PPO) is a resin material with excellent performance, which has excellent low moisture absorption and dimensional stability, and can also maintain extremely low dielectric constant and dielectric loss under high temperature and high frequency environments. Therefore, it has a good application prospect in the field of 5G high-frequency high-speed electronic circuit substrates. In order to enable polyphenylene ether to be better used in the field of high-performance copper clad laminates, it needs to be functionally modified. The introduction of functional groups at both ends of polyphenylene ether is a better solution. It not only has the excellent characteristics of general high molecular weight polyphenylene ether, but als...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08G65/48
CPCC08G65/485C08G2650/04
Inventor 胡冰尚遇青闫亚男陈龙
Owner QINGDAO SANLI BENNUO CHEM IND
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com