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Preparation and application methods of small-grain-size polyimide powder

A polyimide powder and small particle size technology, which is applied in the preparation and application of small particle size polyimide powder, can solve the problems of difficult feeding, uneven particles, high cost, etc., and improve the overall mechanical properties , Simplify the production device and solve the problem of difficult blanking

Active Publication Date: 2019-05-14
CHANGSHA ADVANCED MATERIALS IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing polyimide two-step synthesis method is a commonly used method in industrialization now. Add toluene or xylene to separate water or add acetic anhydride and triethylamine to chemically dehydrate, then precipitate in methanol, ethanol or other solvents, and filter to obtain Polyimide resin, but the polyimide resin obtained by this method is often in the form of flakes or strips, and the particles are not uniform. It needs to be mechanically crushed, sieved and other processes in the later stage to obtain powdered polyimide. Even if the bulk density of the powder obtained in this way is small, the powder is relatively foamy, which makes it difficult to cut the material in the later processing
CN103261277A, CN101253223A disclose the preparation method of polyimide particle, this method needs special ultrasonic equipment, and needs modifier to prepare, and cost is higher, and process is complicated

Method used

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  • Preparation and application methods of small-grain-size polyimide powder

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preparation example Construction

[0027] A preparation method of small particle size polyimide powder, comprising the following steps:

[0028] Dissolve diamine in an organic solvent at room temperature, then add dianhydride to react for 5 hours, add a water separator to raise the temperature to a certain temperature, then pass nitrogen gas and stir for dehydration for 8 hours, then cool down to 90°C, pour the reaction solution into the precipitate while it is hot solution, cooled to normal temperature to crystallize, filtered and dried to obtain resin powder with small particle size, the particle size of polyimide powder is 6μm-15μm. Put the above resin powder into a twin-screw extruder for extrusion granulation, processing temperature: 345°C-360°C, speed: 80r / min-150r / min; Dry in a drying oven for 4 hours, and inject into standard mechanical test specimens by injection molding machine.

Embodiment 1

[0031] Dissolve 20.02g of 4,4'-diaminodiphenyl ether in 167.32g of DMAc at room temperature, slowly add 21.81g of pyromellitic dianhydride, stir and react for 5 hours, then add 33.46g of toluene, blow nitrogen , heated to 155°C and stirred for 8 hours, then cooled to 90°C, poured the reaction solution into 334.64 g of ethanol adjusted to pH 3 with acetic acid, stirred and cooled to room temperature, filtered, and dried at 180°C for 4 hours to obtain a light yellow powder resin , yield 98%. Particle size: D(90)7μm.

Embodiment 2

[0033] Dissolve 24.83g of 4,4'-diaminodiphenylsulfone in 186.56g of NMP at room temperature, slowly add 21.81g of pyromellitic dianhydride, stir and react for 7 hours, then add 37.31g of toluene, and blow argon , heated to 160°C and stirred for 10 hours, then cooled to 80°C, poured the reaction liquid into 373.12 g of methanol whose pH was adjusted to 4 with acetic acid, stirred and cooled to normal temperature, filtered, and dried at 180°C for 4 hours to obtain a light yellow powder resin , yield 97%. Particle size: D(90)6μm.

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Abstract

The invention provides a preparation method of a small-grain-size polyimide powder. The preparation method of the small-grain-size polyimide powder comprises the following steps of dissolving diamineinto organic solvent, then adding in dianhydride for reaction for 3-7 hours, then adding in water separating agent, increasing the temperature to 140-160 DEG C, inletting and mixing in inert gas for dewatering for 6-12 hours, cooling down to 70-90 DEG C, pouring the hot reaction liquid into separated solution, cooling down to 0-35 DEG C for crystallization, and performing filtering and drying to obtain the small-grain-size polyimide powder. The preparation method of the small-grain-size polyimide powder has the advantage that the fine powder is directly obtained after reaction is completed, sothat crushing and screening can be saved, granularity can be uniform, production devices can be simplified, the problem of feeding difficulty during processing can be solved, and industrial values can be achieved. The prepared small-grain-size polyimide powder can be fed into a double-screw extruder for extrusion pelletizing to obtain polyimide granules, which are then injection-molded into standard mechanical testing sample bars for standard mechanical testing, thereby improving the overall mechanical performance.

Description

technical field [0001] The invention relates to a preparation method and application of small-diameter polyimide powder. Background technique [0002] Polyimide is a kind of high-performance polymer containing aromatic ring and imide ring repeating unit structure, which has good mechanical properties and thermal stability. After decades of development, polyimide has developed into a class of high-performance materials with a wide range of products and products, and has always been the focus of research and development in various countries. Especially for its excellent heat resistance and oxidation stability, outstanding mechanical properties at high temperature, radiation resistance and good chemical and physical stability, it has been widely used in many fields such as aerospace, weaponry, automobiles and electronic appliances. application. [0003] The existing polyimide two-step synthesis method is a commonly used method in industrialization now. Add toluene or xylene t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/16C08L79/08C08G73/10
Inventor 刘永亮黄活阳马彦熊平
Owner CHANGSHA ADVANCED MATERIALS IND RES INST CO LTD
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