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Preparation method of polyimide resin

A technology of polyimide resin and polyimide, which is applied in the field of polyimide resin preparation, can solve problems such as difficult recovery of liquid organic water-separating agent and reaction solvent, difficulty in dispersing high-temperature raw materials, etc. Water steps, solving the difficulty of recycling, and the effect of simple process flow

Inactive Publication Date: 2018-04-20
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

[0004] The technical problem solved by the present invention is that the problems of difficult recovery of liquid organic water-separating agent and reaction solvent in the prior art can also solve problems such as high temperature and difficult dispersion of raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 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 2g of silica gel, blow nitrogen, Heat up to 155°C and stir for 8 hours, then cool down to 90°C, filter the reaction solution with suction, stir the filtrate to cool down to room temperature, centrifuge, and dry at 180°C for 4 hours to obtain a light yellow powder resin with a yield of 98%.

Embodiment 2

[0029] Dissolve 24.83g of 4,4'-diaminodiphenylsulfone in 186.56g of NMP at room temperature, slowly add 21.81g of pyromellitic dianhydride, stir for 5 hours, and then add 0.9g of active anhydrous sulfuric acid Copper, blowing nitrogen, heating up to 150°C and stirring for 8 hours, then cooling to 90°C, suction filtering the reaction solution, stirring the filtrate to cool to room temperature, centrifuging, and drying at 180°C for 4 hours to obtain a light yellow powder resin with a yield of 97%.

Embodiment 3

[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 0.5g of molecular sieves, blow nitrogen , heated to 155°C and stirred for 8 hours, then cooled to 90°C, filtered the reaction solution with suction, stirred and cooled the filtrate to room temperature, centrifuged, and dried at 180°C for 4 hours to obtain a light yellow powder resin with a yield of 95%.

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PUM

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Abstract

The invention discloses a preparation method of polyimide resin. The preparation method comprises the following steps: dissolving diamine into an organic solvent and then adding dianhydride for reacting; adding a solid water absorbent for stirring, raising the temperature to 110 to 200 DEG C, introducing nitrogen and continuously reacting for 6 hours or above; then reducing the temperature to be 90 DEG C, separating the solid water absorbent from a reaction liquid in a hot state, reducing the temperature of the reaction liquid to a normal temperature for crystallizing, carrying out solid-liquid separation and drying to obtain the polyimide resin. According to the preparation method of the polyimide resin, disclosed by the invention, a liquid dehydrating agent is substituted with the solidwater absorbent, a production device is simplified, and the problem that a mixed solution is difficult to recover is solved; the solid water absorbent can be recycled and reused, a reaction solvent asfiltrate can be recycled and the technical process is simple; the polyimide resin has an industrialized value.

Description

technical field [0001] The invention relates to a preparation method of polyimide resin. 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] Existing polyimide synthesis techniques and technologies include melt polymerization, supercritical carbon dioxide polymerization, aqueous phase synthesis, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC08G73/1007C08G73/1064C08G73/1071
Inventor 刘永亮王洋黄活阳周利庄
Owner CHANGSHA ADVANCED MATERIALS IND RES INST CO LTD
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