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Method for preparing poly(arylene ether nitrile) resin

A technology of polyarylether nitrile and resin, which is applied in the field of preparation of polyarylether nitrile resin, can solve the problems of solvent not being recovered and recycled by rectification, high reaction temperature and pressure, and limited application range of resin, etc., to overcome side effects Effects of reactions and by-products, stable performance, and easy-to-achieve production conditions

Active Publication Date: 2011-12-21
SICHUAN FEIYA NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] There are three deficiencies in the production methods described in these patents: the one is that the reaction temperature and the reaction pressure are relatively high (the reaction temperature reaches 180~300 ℃, and the reaction pressure reaches 2~5MPa); In this purification method, the purity of the product is low due to the fact that some inorganic salt particles are still wrapped in the resin, which limits the application range of the resin; the third is that the solvent is not recycled by rectification, resulting in increased raw material costs and environmental pollution

Method used

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  • Method for preparing poly(arylene ether nitrile) resin
  • Method for preparing poly(arylene ether nitrile) resin
  • Method for preparing poly(arylene ether nitrile) resin

Examples

Experimental program
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Effect test

Embodiment 1

[0022] According to the following molar ratio: 2,6-dichlorobenzonitrile: hydroquinone: resorcinol: anhydrous potassium carbonate: N-methylpyrrolidone: toluene = 1: 0.9: 0.1: 1.2: 6: 1.3 Weigh the raw materials and put them into the reaction kettle, heat and stir to 140°C for dehydration reaction, during the dehydration reaction process, the water generated by the reaction is separated by the reflux device, and the toluene is refluxed; after the dehydration reaction for 2 hours, the reaction system is heated to 200°C under normal pressure The N-methylpyrrolidone solvent injected into the reactor dilutes the solution until the polymer climbing rod phenomenon occurs during the polymerization reaction until the viscosity of the solution is less than 2000 centipoise. The diluted solution system is sprayed into a precipitation tank with a precipitating agent in a pressurized spraying manner, then heated and stirred, fully refluxed and separated from solid and liquid by a centrifuge, ...

Embodiment 2

[0026] According to the following molar ratio: 2,6-dichlorobenzonitrile: biphenol: anhydrous potassium carbonate: N-methylpyrrolidone: toluene = 1: 1: 1.3: 7: 1.4 Weigh the raw materials and put them into the reactor During the dehydration reaction, heat and stir to 150°C for dehydration reaction. During the dehydration reaction, the water generated by the reaction is separated by the reflux device, and the toluene is refluxed; after the dehydration reaction for 3 hours, the temperature of the reaction system is raised to 200°C, and the polymerization reaction is carried out under normal pressure until polymers appear. When the rod climbing phenomenon occurs, the N-methylpyrrolidone solvent injected into the reactor dilutes the solution until the viscosity of the solution is less than 2000 centipoise. The diluted solution system is sprayed into a precipitation tank with a precipitating agent in a pressurized spraying manner, then heated and stirred, fully refluxed and separated...

Embodiment 3

[0031] According to the following molar ratio: 2,6-dichlorobenzonitrile: bisphenol A: anhydrous potassium carbonate: N-methylpyrrolidone: toluene = 1: 1: 1.2: 6: 1.3 Weigh the raw materials and put them into the reaction kettle , heated and stirred to 140°C for dehydration reaction. During the dehydration reaction, the water generated by the reaction was separated by the reflux device, and the toluene was refluxed; When rod phenomenon occurs, the N-methylpyrrolidone solvent injected into the reactor dilutes the solution until the solution viscosity is less than 2000 centipoise. The diluted solution system is sprayed into a precipitation tank with a precipitating agent in a pressurized spraying manner, then heated and stirred, fully refluxed and separated from solid and liquid by a centrifuge, and the separated liquid is sent to a rectification tower to rectify and recover the solvent In order to be recycled; the separated solid is firstly washed and filtered with acidic boilin...

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Abstract

The invention discloses a method for preparing poly(arylene ether nitrile) resin, which belongs to the technical field of high polymer materials. The method comprises the following steps of: finishing a reaction in a reaction kettle under normal pressure under the actions of a catalyst and a dehydrating agent by taking 2,6-dichlorobenzonitrile and aromatic dicarboxylic phenol as raw materials andtaking N-methyl pyrrolidone as a solvent; pressurizing and atomizing solution after dilution to a precipitating agent for precipitating; after heating, stirring and refluxing a precipitate and the precipitating agent to finish solvent extraction, performing solid-liquid separation by using a centrifugal machine; allowing liquid to enter a rectifying tower for rectifying and recovering the solvent; and drying solid after washing with boiling water to obtain the poly(arylene ether nitrile) resin of the invention. The method has the characteristics of easily implemented production conditions, and safe and environmentally-friendly production process. The poly(arylene ether nitrile) resin prepared by adopting the method of the invention has the characteristics of high purity and stable performance, and can be applied to the field of aerospace, electronics, machinery, medical treatment, chemical industry and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a preparation method of polyarylether nitrile resin Background technique [0002] Polyarylether nitrile is a kind of thermoplastic polymer with nitrile groups on the side chain. It is a kind of high-performance structure with excellent comprehensive performance developed for the needs of national defense and military industry and cutting-edge technology since the 1980s. Molecular materials, with high heat resistance, flame retardancy, mechanical strength, UV protection and creep resistance, can be widely used in aerospace, electronic packaging, machinery manufacturing, auto parts and other fields, [0003] The domestic research on poly(arylene ether nitrile) started in the 1980s, mainly focusing on the research of synthesis process and formulation. Domestic invention patents on polyarylether nitrile resins mainly include: "A Polyarylether Nitrile and Its Manufacturing Me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/40C08G65/46
Inventor 钟家春刘孝波杨建孟凡彬赵睿
Owner SICHUAN FEIYA NEW MATERIAL
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