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Preparation method for amination polyphenyl ether

A polyphenylene ether, amination technology, used in plastic/resin/wax insulators, organic insulators, etc., can solve problems such as increasing industrialization and environmental protection, and achieve excellent mechanical properties, electrical properties, and compatibility.

Active Publication Date: 2013-06-05
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nitro- and amino-modified polyphenylene ethers can not only maintain the mechanical properties of polyphenylene ethers, but also improve the compatibility of polyphenylene ethers with polar polymers. However, this method not only uses toxic chloroform solvents, but also uses Severely corrosive concentrated sulfuric acid and concentrated nitric acid increase the difficulty of industrialization and environmental protection

Method used

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  • Preparation method for amination polyphenyl ether
  • Preparation method for amination polyphenyl ether
  • Preparation method for amination polyphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] In a reactor equipped with a reflux condenser, stirring, and a thermocouple, 1.35 g (0.0061 mol) of copper bromide, 6.34 g (0.0491 mol) of dibutylamine, and 1180 g of methanol were added successively, and complexed at room temperature for 10 min. Add 116g (0.409mol) 3,3,5,5-tetramethylbisphenol A and 200g (1.637mol) 2,6-dimethylphenol, (the molar ratio of the two monomers is 1:4,) to maintain the temperature At 25°C, under the condition of vigorous stirring, air was introduced at a speed of 1.637 NL / min, and the reaction was carried out for 2 hours. Terminate the reaction with 1 mL of acetic acid with a concentration of 1 mol / L, filter, then wash with deionized water, methanol, and dry to obtain 230 g of white powder, which is PPO-2OH, with a yield of 73%. Mn=1507g / mol, Mw=2828g / mol, D=1.87 measured by GPC (gel permeation chromatography).

Embodiment 2

[0056] In a reactor equipped with a reflux condenser, stirring, and a thermocouple, 2.024g (0.009mol) of copper bromide, 4.43g (0.09822mol) of dimethylamine, and 3681g of ethanol were added successively, and complexed at room temperature for 10min. Add 209.4g (0.818mol) 3,3,5,5-tetramethylbisphenol F and 200g (1.637mol) 2,6-dimethylphenol, (the molar ratio of the two monomers is 1:2,) keep The temperature was 60°C, under the condition of vigorous stirring, air was introduced at a speed of 0.2 NL / min, and the reaction was carried out for 2.5 hours. Terminate the reaction with 1 mL of oxalic acid with a concentration of 1 mol / L, filter, then wash with deionized water, methanol, and dry to obtain 227.6 g of white powder, which is PPO-2OH, with a yield of 55.5%. Mn=1031 g / mol, Mw=1912 g / mol, D=1.85 were measured by GPC.

Embodiment 3

[0058] In a reactor equipped with a reflux condenser, stirring and thermocouple, add 0.5485g (0.0025mol) of copper bromide, 1.8g (0.0246mol) of diethylamine, 782g of 40% methanol and 60% ethanol in sequence mixed solvent, complexed at room temperature for 10min, added 34.8g (0.1227mol) 3,3,5,5-tetramethylbisphenol A and 300g (2.456mol) 2,6-dimethylphenol, (two mono The volume molar ratio is 1:20,) keeping the temperature at 10°C, under the condition of vigorous stirring, the air was passed in at a speed of 0.082NL / min, and the reaction was carried out for 10h. Terminate the reaction with 1 mL of hydrochloric acid with a concentration of 1 mol / L, filter, wash with deionized water, methanol, and dry to obtain 286 g of white powder, which is PPO-2OH, with a yield of 85.4%. Mn=2631 g / mol, Mw=5098 g / mol, D=1.94 were measured by GPC.

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Abstract

The invention discloses a preparation method for amination polyphenyl ether, which is characterized by including the following steps that low-molecular-weight polyphenyl ether with double hydroxyl is generated through oxidation, coupling and copolymerization of two kinds of phenol, and low-molecular-weight polyphenyl ether resin with double amino is obtained through a process such as nitration. Compared with conventional polyphenyl ether resin, the polyphenyl ether resin with the double amino is more in active groups cross-linked with epoxy, larger in cross-linking degree with epoxy resin, can remarkably improve poly-p-phenylene oxide / epoxy (PPO / EP) compatibility, can increase proportion of the polyphenyl ether resin in a PPO / EP system, and accordingly remarkably improves condensate electrical property of a resin system.

Description

technical field [0001] The invention belongs to the preparation of polymer materials, and relates to a preparation method of aminated polyphenylene ether. The prepared aminated polyphenylene ether is suitable for use as a resin modifier for insulating materials in electrical and electronic products. Background technique [0002] Epoxy resin (EP) has many excellent properties and good cost performance and is widely used, but epoxy resin also has defects such as brittleness and poor electrical performance, so it is limited in some high-end fields such as high-performance electronic and electrical products. , Applications in automotive products. To expand its scope of application, it must be modified. [0003] Polyphenylene ether resin (PPO) is a thermoplastic engineering plastic with excellent performance. It has high mechanical strength and heat resistance, good dimensional stability, low moisture absorption rate, dielectric constant and dielectric loss are almost independe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/48C08G65/44C08L63/00C08L71/12H01B3/40
Inventor 代三威李建学黄洪驰李先德
Owner SICHUAN DONGFANG INSULATING MATERIAL
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