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A kind of preparation method of polyphenylene ether

A polyphenylene ether and polymer technology, applied in the field of engineering material polyphenylene ether preparation, can solve the problems of high toxicity, environmental pollution, low yield, etc.

Active Publication Date: 2020-12-25
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The traditional synthesis method of polyphenylene ether uses copper amine catalyst, highly toxic nitrobenzene or toluene as solvent, and oxygen or hydrogen peroxide as oxidant to synthesize polyphenylene ether. This method not only has high cost and low yield, but also has high toxicity. , will cause great pollution to the environment, this method is still the mainstream method of synthesizing polyphenylene ether

Method used

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  • A kind of preparation method of polyphenylene ether
  • A kind of preparation method of polyphenylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Put 2.23g (10mmol) of copper bromide into a PTFE-lined autoclave, add an appropriate amount of ethanol, mix well, cover the lid tightly, place in a muffle furnace, control the temperature at 200°C, and react for 18 hours . After the reaction is completed, take out the reaction kettle, cool to room temperature, vacuum filter under reduced pressure, wash with ethanol, and vacuum-dry the product obtained by suction filtration to obtain nano-cuprous bromide. Weigh nano-cuprous bromide (0.1g) into a four-necked flask, then add dimethyl n-butylamine (4mL), the molar ratio of nano-cuprous bromide and dimethyl n-butylamine is 1:50, The color becomes pale yellow, then add 30ml of tetrahydrofuran as solvent, the color turns to yellow-green, put the device on the magnetic stirrer, start stirring and let oxygen into the oxygen for 5 minutes, then add 2.2ml of tetrahydrofuran into the four-necked flask 2,6-Xylenol (2.5g, 18mmol), continue to feed oxygen for 2 hours, after reacting ...

Embodiment 2

[0028] According to the method and operation steps of Example 1, the process of introducing oxygen in Example 1 was changed to the process of introducing air to obtain 1.87 g of light yellow polyphenylene ether with a yield of 74.80%. It can be seen that replacing oxygen with air does not have much influence on the yield and quality of polyphenylene ether.

Embodiment 3

[0030] According to the method and operation steps of Example 2, the nano-sized cuprous bromide in Example 2 was changed to commercial cuprous bromide to obtain 1.03 g of light yellow polyphenylene ether with a yield of 41.20%. It can be seen that the catalytic activity of nano-sized cuprous bromide provided by the present invention is much higher than that of commercial cuprous bromide by adopting the process of feeding air.

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Abstract

The invention provides an efficient, environment-friendly and low-cost preparation method for an engineering material, namely polyphenyl ether (PPO). According to the preparation method, cuprous bromide nanoparticles are prepared from copper bromide, organic amine and nano-scale cuprous bromide are taken as a copper amine catalyst, and tetrahydrofuran is taken as a solvent, so that high cost caused due to the use of oxygen or hydrogen peroxide is saved in a whole-process air introduction manner, the polymerization reaction of 2,6-dimethylaminophenol is realized, the yield is substantially increased, the environmental influence is minimized, and the production cost is greatly lowered.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a method for preparing an efficient, green and low-cost engineering material polyphenylene ether. Background technique [0002] The oxidative polymerization of 2,6-dimethylphenol (DMP) catalyzed by copper-amine complexes was first discovered by AS Hay in 1959 using CuCl-pyridine complexes as catalysts in oxygen. This reaction synthesizes polyphenylene oxide (PPO) via CO coupling, as shown in Equation 1. However, cuprous chloride is an extremely unstable cuprous salt, and catalytic deactivation will occur during transportation, storage, feeding and other processes. Polyphenylene ether is an important engineering thermoplastic used in many industrial applications due to its high thermal stability, low water absorption and chemical resistance. [0003] [0004] Polyphenylene oxide (PPO) is a thermoplastic engineering plastic with excellent performance, because it has th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/44
CPCC08G65/44
Inventor 班鑫鑫陈枫潘杰刘艳朱爱云张源源张田林童志伟
Owner HUAIHAI INST OF TECH
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