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Preparation method of polyarylene ether nitrile resin

A polyarylether nitrile and resin technology, applied in the field of polymer material synthesis, can solve the problems of low utilization rate of equipment, incomplete formation of phenate, large amount of solvent, etc., to reduce the recovery cost of solvent, reduce synthesis cost, reduce The effect of usage

Active Publication Date: 2019-09-20
YIBIN TIANYUAN GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method has the following disadvantages (1) when the polymerization, the solid content is about 30%-35%, and the production of one ton of polyarylether nitrile needs to add 2.3-2.6 tons of N-methylpyrrolidone. Under the same equipment conditions, polyarylether nitrile The production capacity of resin is low, and the utilization rate of equipment is low; (2) The amount of solvent to be recovered is large, which increases the cost of solvent recovery; (3) The content of dehydrating agent and salt in the product is high, which affects the purification process and quality of the product
According to the traditional method of synthesizing polyarylether nitrile, if the solid content is directly increased, there will be problems that high molecular weight polymers cannot be obtained due to difficult dehydration reactions and incomplete formation of phenoxides.
One reason may be that under the condition of high solid content, the alkali metal salt is encapsulated by the generated phenoxide, resulting in incomplete dehydration reaction, and at the same time, the catalytic efficiency of the catalyst is reduced because the alkali metal salt is encapsulated by the generated phenoxide

Method used

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  • Preparation method of polyarylene ether nitrile resin
  • Preparation method of polyarylene ether nitrile resin
  • Preparation method of polyarylene ether nitrile resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A preparation method of polyarylether nitrile resin, comprising the following steps:

[0038] (a) Prepare materials with the molar ratio of bisphenol A, potassium hydroxide and toluene as 1:2.05:6, and prepare potassium hydroxide solution with a mass fraction of 30%; put bisphenol A and toluene into nitrogen gas In the reactor protecting and condensing the water separator, raise the temperature to 80°C, after the bisphenol A is dissolved, raise the temperature to 120°C, control the potassium hydroxide solution to drop into the reactor within 55±5min, and form a salt After 2 hours of reaction, the water and toluene in the system are azeotroped. After the azeotropic gas is cooled by the condenser, it is layered in the water separator to remove water. After the salt formation reaction is completed, all the toluene is evaporated, and after vacuum drying, bisphenol is obtained. A potassium salt;

[0039] (b) Put bisphenol A potassium salt, 2,6-dichlorobenzonitrile, N-methyl...

Embodiment 2

[0043] A preparation method of polyarylether nitrile resin, comprising the following steps:

[0044] (a) Prepare materials with the molar ratio of bisphenol A, potassium hydroxide and xylene as 1:2.05:4, and potassium hydroxide is prepared into a potassium hydroxide solution with a mass fraction of 20%; put bisphenol A and xylene into In the reaction kettle with nitrogen protection and condensation water separator, raise the temperature to 110°C, after the bisphenol A is dissolved, raise the temperature to 140°C, control the potassium hydroxide solution to drop into the reactor within 40±5min, Salt-forming reaction for 2 hours, the water in the system and xylene are azeotropic, after the azeotropic gas is cooled by a condenser, it is layered in a water separator to remove water, after the completion of the salt-forming reaction, all the xylene is evaporated, and after vacuum drying That is, bisphenol A potassium salt;

[0045] (b) Put bisphenol A potassium salt, 2,6-dichlorob...

Embodiment 3

[0049] A preparation method of polyarylether nitrile resin, comprising the following steps:

[0050] (a) with the mol ratio of bisphenol A, potassium hydroxide and mesitylene as 1: 2.05:5 to prepare raw materials, potassium hydroxide is mixed with the potassium hydroxide solution that mass fraction is 40%; Bisphenol A, mesitylene drop into In the reactor with nitrogen protection and condensing water separator, raise the temperature to 140°C, after the bisphenol A is dissolved, raise the temperature to 180°C, control the potassium hydroxide solution to drop into the reactor within 35±5min, Salt formation reaction 2.5h, the water in the system and trimethylbenzene azeotrope, after the azeotropic gas is cooled by the condenser, layered in the water separator to remove water, after the completion of the salt formation reaction, evaporate all the xylene, vacuum dry After that, bisphenol A potassium salt is obtained;

[0051] (b) Put bisphenol A potassium salt, 2,6-dichlorobenzonitri...

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Abstract

The invention belongs to the technical field of high polymer materials, and particularly discloses a method for synthesizing polyarylene ether nitrile resin under the condition of high solid content, which specifically comprises the following steps: firstly, performing a reaction on bisphenol A with an alkali solution to obtain phenol-alkali salt of bisphenol A; drying the phenol-alkali salt and polymerizing the phenol-alkali salt with 2,6-dichlorobenzonitrile and alkali carbonate with a small amount of N-methylpyrrolidone being a solvent to generate a high-molecular polymer; and finally crushing, purifying and drying the polymer to obtain the polyarylene ether nitrile resin product. In the polyarylene ether nitrile prepared by the method, the content of benzene series, such as toluene and xylene, is low; in the preparation process, the dosage of N-methylpyrrolidone is reduced, and the synthesis cost of the polyarylene ether nitrile resin and the recovery cost of the N-methyl pyrrolidone are reduced, so that the equipment utilization rate, the product quality and the economic benefit are improved.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis and specifically discloses a method for preparing polyarylether nitrile resin under the condition of high solid content. Background technique [0002] Polyarylene ether nitrile (PEN) is a thermoplastic polymer with aromatic ether structural units in the main chain of the macromolecule, and one of the aromatic ether side groups is a nitrile group; it has good thermal stability, high mechanical properties, good insulation, and chemical resistance. It has excellent comprehensive properties such as product corrosion and self-flame retardancy; it is widely used in electronic appliances, machinery manufacturing, auto parts, aerospace and other fields. [0003] At present, the synthetic method that prepares polyarylether nitrile mainly adopts is by dihalogenated benzonitrile and dihydric phenol in polar solvents such as N-methylpyrrolidone (NMP), with carbonate as catalyst, toluene as dehydratin...

Claims

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Application Information

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IPC IPC(8): C08G65/40
CPCC08G65/4006
Inventor 邓敏高在平谢濠江缑可贞徐慧远
Owner YIBIN TIANYUAN GRP CO LTD