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A kind of synthetic preparation method of polybenzimidazole resin

A technology for polybenzimidazole and resin, which is applied in the field of synthesis and preparation of polybenzimidazole resin, can solve problems such as being unsuitable for industrial production, high temperature and high pressure, and achieve the effects of improving processability, increasing the degree of polymerization and molecular weight

Active Publication Date: 2021-06-01
常州源自然新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problems existing in the prior art that the reaction requires high temperature and high pressure and is not suitable for industrial production, the invention provides a method for the synthesis and preparation of polybenzimidazole resin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 100 g of 4,4'-diaminodiphenyl ether with a molar mass of 0.5 mol and 600 g of glacial acetic acid with a molar mass of 10 mol into a 2L four-neck flask, heat and reflux for 8-10 hours, and use thin-layer chromatography to track the complete reaction of the raw materials. The developing agent used and its proportioning ratio are: ethyl acetate: n-hexane = 5:1, no need to process, directly cool to below 50°C, add dropwise 100g of nitric acid with a concentration of 65% and a molar mass of 1.5mol in the system, After the dropwise addition, the temperature was continued for 2 hours, and then the reaction solution was poured into 2000ml of water to precipitate a solid, washed with water, and dried to obtain 140g of a solid.

[0029] Then the obtained solid, 100g of water, 30ml of hydrochloric acid with a concentration of 30%, and 600ml of ethanol with a concentration of 95% were added together in a 2L four-necked bottle and heated to reflux until the raw materials were co...

Embodiment 2

[0032] Add 100 g of 4,4'-diaminodiphenyl ether with a molar mass of 0.5 mol and 600 g of glacial acetic acid with a molar mass of 10 mol into a 2L four-neck flask, heat and reflux for 8-10 hours, and use thin-layer chromatography to track the complete reaction of the raw materials. The developing agent used and its proportioning ratio are: ethyl acetate: n-hexane = 5:1, no need to process, directly cool to below 50°C, add dropwise 100g of nitric acid with a concentration of 65% and a molar mass of 1.5mol in the system, After the dropwise addition, the temperature was continued for 2 hours, and then the reaction solution was poured into 2000ml of water to precipitate a solid, washed with water, and dried to obtain 140g of a solid.

[0033] Then the obtained solid, 100g of water, 30ml of hydrochloric acid with a concentration of 30%, and 600ml of ethanol with a concentration of 95% were added together in a 2L four-necked bottle and heated to reflux until the raw materials were co...

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Abstract

The invention provides a method for synthesizing and preparing polybenzimidazole resin, comprising the following steps: Step 1: Add 300ml of PPA and 46g of 3,3',4,4'-tetraaminodiphenyl ether into a dry four-necked bottle , 1,4 naphthalene dicarboxylic acid or 2,6-naphthalene dicarboxylic acid 43g, crosslinking agent 2,6-pyridine dicarboxylic acid 33g; Step 2: feed nitrogen into the four-necked bottle of step 1, then slowly heat and heat up to a certain temperature and keep it warm for a period of time; step 3: then heat again, raise the temperature to a certain temperature and keep it warm for a period of time; step 4: then pour the reaction solution obtained in step 3 into deionized water, stir to precipitate a reddish-brown solid; step 5 : the reddish-brown solid obtained in step 4 is suction-filtered, then soaked with sodium bicarbonate solution for a certain period of time, then washed out with deionized water, and finally dried to obtain the polybenzimidazole resin.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a method for synthesizing and preparing polybenzimidazole resin. Background technique [0002] With the development of aerospace technology, especially the improvement of the flight speed of spacecraft and the ratio of payload to structure mass, high temperature resistant advanced composite materials are becoming the most important new aerospace structural materials. Polybenzimidazole (PBI) still has good mechanical, electrical, self-lubricating, radiation resistance, hydrolysis resistance, flame retardancy and burning resistance at 400 °C. Polybenzimidazole (PBI) resin glass fiber laminated material has good high temperature bending strength at 425°C, and has been applied in radome, fairing and empennage of supersonic aircraft, burn-resistant coating, and radiation resistance of spacecraft Materials, printed circuit boards, C-level electrical insulation materials and FPC ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/18
CPCC08G73/18
Inventor 蔡旭光
Owner 常州源自然新材料科技有限公司
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