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Method for preparing poly(arylene ether nitrile) resin powder

A polyarylether nitrile and resin powder technology, which is applied in the field of polyarylether nitrile resin powder and its preparation, can solve the problems of complex preparation process, insufficient purity, and reduced resin performance, and achieve excellent electrical properties, uniform particle size, and high performance stable effect

Active Publication Date: 2011-01-19
SICHUAN FEIYA NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the purification methods of these polyarylether nitrile resins all adopt mechanical crushing and washing with boiling water. The mechanical crushing method to prepare polyarylether nitrile resin powder mainly has the following three shortcomings: the first is that the molecular chain of the resin will be destroyed to a certain extent through powerful crushing , thereby reducing the performance of the resin; the second is that because the polyarylether nitrile resin has good toughness, it is difficult to grind the resin evenly to 100 mesh powder by mechanical pulverization, which makes it difficult to purify the inorganic salt particles wrapped in the resin. Thereby affecting the stability of the performance and the scope of application; the third is that mechanical pulverization is difficult to operate in a fully enclosed and continuous manner, which is not conducive to environmental protection
The polyarylether nitrile resin powder obtained by this method has poor particle uniformity, resulting in insufficient purity; and the need for pressurized spraying in the preparation process makes the preparation process more complicated

Method used

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

Examples

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Effect test

Embodiment 1

[0025] Molar ratio: 2,6-dichlorobenzonitrile: hydroquinone: resorcinol: anhydrous potassium carbonate: N-methylpyrrolidone: toluene = 1:0.9:0.1:1.2:6:1.3 preparation Raw materials are put into a reaction kettle with water separator, agitator and heater, and the temperature is raised to 140°C for dehydration reaction for 2 hours under stirring. Toluene is evaporated through the water separator, and the temperature is raised to 200°C. When rod phenomenon occurs, a certain amount of N-methylpyrrolidone solvent is injected into the reactor to terminate the reaction, and at the same time, the reaction solution is diluted so that the mass concentration of the reaction product is 2-10%. Cool down the temperature in the reactor to 120-140°C and add ethanol to the reactor. The amount of ethanol added is 70-110% of the volume of N-methylpyrrolidone. The temperature in the reactor is controlled at 20-70°C. After continuous stirring for 1 hour, Centrifuge for solid-liquid separation, put ...

Embodiment 2

[0029] Molar ratio: 2,6-dichlorobenzonitrile: biphenol: anhydrous potassium carbonate: N-methylpyrrolidone: toluene = 1: 1: 1.3: 7: 1.4 Prepare the raw materials and put them into the belt In the reaction kettle with water tank, agitator and heater, heat and stir to 150°C for dehydration reaction for 2 hours, steam the toluene through the water separator, raise the temperature to 200°C, and inject it into the reaction kettle when the rod climbing phenomenon occurs. A certain amount of N-methylpyrrolidone solvent terminates the reaction, so that the mass concentration of the reaction product is 8-15%. Lower the temperature in the reactor to 120-140°C and add methanol to the reactor. The amount of methanol added is 50-80% of the volume of N-methylpyrrolidone. The temperature in the reactor is controlled at 20-100°C. After continuous stirring for 1 hour, the Centrifuge for solid-liquid separation, put the solid into oxalic acid or hydrochloric acid boiling aqueous solution with a...

Embodiment 3

[0033]Molar ratio: 2,6-dichlorobenzonitrile: bisphenol A: anhydrous potassium carbonate: N-methylpyrrolidone: toluene = 1: 1: 1.2: 6: 1.3 Prepare raw materials, and put into Heating and stirring to 140°C for dehydration reaction for 3 hours, steaming toluene through the water separator, raising the temperature to 200°C, and injecting a certain amount of A certain amount of N-methylpyrrolidone solvent terminates the reaction, so that the mass concentration of the reaction product is 10-15%. Cool down the temperature in the reaction kettle to 120-140°C and add water to the reaction kettle. The amount of water added is 130-200% of the volume of N-methylpyrrolidone. The temperature in the reaction kettle is controlled at 20-70°C. After continuous stirring for 1 hour, Centrifuge for solid-liquid separation, put the solid into oxalic acid or hydrochloric acid boiling aqueous solution with a pH value between (5,7), wash three times, filter, and then dry at 150°C for 8 hours to obtain...

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Abstract

The invention discloses a method for preparing poly(arylene ether nitrile) resin powder, and belongs to the technical field of high polymer materials. 2,6-dichlorobenzonitrile and aromatic dihydric phenol are taken as raw materials, 1-methyl-2-Pyrrolidinone is taken as a solvent, anhydrous potassium carbonate or anhydrous sodium carbonate is taken as a catalyst, and methylbenzene or dimethylbenzene is taken as a dehydrating agent; and the method comprises the following steps of: performing reflux reaction at the temperature of between 130 and 160 DEG C for 2 to 4 hours in a reactor, slowly evaporating out water and the dehydrating agent, and raising the temperature to 180-200 DEG C until a macromolecular rod-climbing phenomenon happens; adding the solvent into the reactor, and diluting the reaction products to the mass concentration of 2 to 15 percent; and adding a precipitator into the reactor, continuously stirring, performing centrifugal solid-liquid separation, washing the solid in acidic boiling water, filtering and drying to obtain the poly(arylene ether nitrile) resin powder. The prepared poly(arylene ether nitrile) resin powder has the characteristics of superfine granularity (reaching 100-400 meshes), uniform granularity, high purity, stable performance, and excellent electrical property, and can be widely applied in the fields such as electronics, precision machines, aerospace, new energy and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to polyarylether nitrile resin powder and a preparation method thereof. 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 have excellent properties such as high heat resistance, flame retardancy, mechanical strength, UV protection and creep resistance, and 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 synthesis process and formula. Domestic applications for the production invention patents of polyarylether nitrile resin m...

Claims

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Application Information

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IPC IPC(8): C08G65/40C08G65/46C08J3/12
Inventor 钟家春杨建赵睿刘孝波
Owner SICHUAN FEIYA NEW MATERIAL
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