Polyimide resin and its preparation method

A technology of polyimide resin and polymerization degree, which is applied in the field of polyimide resin and its preparation, can solve the problems of poor fluidity and poor temperature resistance of polyimide resin, and achieve the purpose of maintaining temperature resistance and improving resistance flammability, fluidity improvement effect

Active Publication Date: 2017-12-01
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 polyimide resin has poor fluidity and poor temperature resistance

Method used

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  • Polyimide resin and its preparation method
  • Polyimide resin and its preparation method
  • Polyimide resin and its preparation method

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preparation example Construction

[0043] The preparation method of polyimide resin generally comprises the following steps:

[0044] 1) Dissolve the hydroxyl compound and the basic compound in an organic solvent and react at room temperature for 2-3 hours, then add 4,4'-dichlorodiphenyl sulfone and raise the temperature to 150°C for 4-5 hours, cool down to room temperature, and then add methane React the aminophenol for 2-3 hours, add a dehydrating agent, then heat up to 140-160°C for dehydration, evaporate the dehydrating agent, and obtain a flexible diamine monomer solution;

[0045] 2) Add pyromellitic dianhydride to the flexible diamine monomer solution obtained in 1) and react at room temperature for 5-7 hours, then add a dehydrating agent at 140-160°C for azeotropic dehydration for 4-6 hours, and pour the reaction solution into the eluent, filtered, washed, and air-dried at 100°C for 4 hours to obtain a polyimide resin.

[0046] The thermal decomposition temperature of 5% weight loss is measured by a th...

Embodiment 1

[0051] Add 36.6g of compound A and 16g of sodium hydroxide to 463.4g of DMAc, stir at room temperature for 2.5 hours, then slowly add 57.43g of 4,4'-dichlorodiphenyl sulfone, raise the temperature to 150°C for 4 hours, drop to After reaching room temperature, 21.82g m-aminophenol was added, stirred for 3 hours, then 92.68g xylene was added, the temperature was raised to 150°C for reflux dehydration for 4 hours, and the xylene was distilled off to obtain a flexible diamine monomer solution.

[0052] After the above flexible diamine monomer solution has dropped to room temperature, slowly add 23.99g of pyromellitic dianhydride, stir and react for 6 hours, then add 92.68g of xylene, heat up to 150°C for reflux dehydration for 5 hours, and pour the reaction solution into In 500g of ethanol, filter, then wash three times with 500g of ethanol, 100 ℃ of blast drying 4 hours, obtain yellow powder resin 116.8g, yield 96%, 5% mass loss thermal decomposition temperature 550 ℃, minimum mel...

Embodiment 2

[0054] Add 36.6g of compound A and 16g of sodium hydroxide to 463.4g of NMP, stir at room temperature for 2.5 hours, then slowly add 57.43g of 4,4'-dichlorodiphenyl sulfone, raise the temperature to 150°C for 4 hours, drop to After reaching room temperature, 21.82g m-aminophenol was added, stirred for 3 hours, then 92.68g xylene was added, the temperature was raised to 150°C for reflux dehydration for 4 hours, and the xylene was distilled off to obtain a flexible diamine monomer solution.

[0055] After the above flexible diamine monomer solution has dropped to room temperature, slowly add 23.99g of pyromellitic dianhydride, stir and react for 6 hours, then add 92.68g of xylene, heat up to 150°C for reflux dehydration for 5 hours, and pour the reaction solution into In 500g of ethanol, filter, then wash three times with 500g of ethanol, 100 ℃ of blast drying 4 hours, obtain yellow powder resin 113.1g, yield 93%, 5% mass loss thermal decomposition temperature 556 ℃, minimum melt...

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Abstract

The invention discloses a polyimide resin and its preparation method. The structural formula of the polyimide resin includes the following structure unit: the structure is as shown in the formula. A diamine monomer containing flexible chain section is autonomously compounded, and the flexible chain section is introduced to the polyimide resin; thus the resin mobility is improved; meanwhile, phosphorus element is introduced, and the temperature resistance of resin is kept; moreover, the flame retardance of resin is improved.

Description

technical field [0001] The invention relates to a polyimide resin and a preparation method thereof. Background technique [0002] Polyimide is a class of high-performance polymers containing repeating structural units of aromatic rings and imide rings, and 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] However, due to the rigidity of the polyimide molecular chain and the strong interaction between the molecules, the ordinary polyimide res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C07F9/09
CPCC07F9/091C08G73/1007C08G73/1057C08G73/1064C08G73/1071
Inventor 王洋刘永亮李真真李江罗熙雯周利庄
Owner CHANGSHA ADVANCED MATERIALS IND RES INST CO LTD
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