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Naphthalene structure-containing high heat-resistant hyperbranched polyimide as well as preparation method and application thereof

A technology of polyimide and polyimide film, applied in the field of material science, can solve the problems of limited wide application, large inter-chain distance, decreased heat resistance, etc., to achieve good application prospects, improve thermal properties, free volume increased effect

Inactive Publication Date: 2018-12-11
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Compared with linear polyimide materials, the distance between hyperbranched polyimide molecular chains is large, which improves its solubility, but its heat resistance is relatively reduced, which limits its application in aerospace, aerospace vehicle structures or functional parts and Wide application in the field of parts and components of rockets, missiles, etc.

Method used

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  • Naphthalene structure-containing high heat-resistant hyperbranched polyimide as well as preparation method and application thereof
  • Naphthalene structure-containing high heat-resistant hyperbranched polyimide as well as preparation method and application thereof
  • Naphthalene structure-containing high heat-resistant hyperbranched polyimide as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 0.4362g (2mmol) of pyromellitic dianhydride (PMDA) and 36ml of N,N-dimethylformamide into a three-necked flask, blow in argon, raise the temperature to 30°C, and add the triamine monomer N 1 -(4-aminophenyl)-N 1 -(3-(4-aminophenyl)naphthalen-1-yl)benzene-1,4-diamine 0.4165g (1mmol) dissolved in 40ml N,N-dimethylformamide with a constant pressure dropping funnel in 1 ~ 2h Add it dropwise into a three-necked flask, then continue to react for 15 hours, then add 6ml of acetic anhydride and 2ml of triethylamine, heat up to 45°C and continue to react for 12 hours, after the reaction is completed, cool to room temperature and discharge in methanol, filter, wash, repeat 2-3 Finally, place it in a vacuum drying oven at 80°C for 24 hours to obtain a brown hyperbranched polyimide polymer, whose structural formula is as follows:

[0038]

Embodiment 2

[0040] Add 0.4515g (2.07mmol) of pyromellitic dianhydride (PMDA) and 15ml of N,N-dimethylacetamide into a three-necked flask, blow in argon, raise the temperature to 30°C, and add the triamine monomer N 1 -(4-aminophenyl)-N 1 -(8-(4-aminophenyl)naphthalen-1-yl)benzene-1,4-diamine 0.4165g (1mmol) dissolved in 16ml of N,N-dimethylacetamide with a constant pressure dropping funnel in 1 ~ 2h Add it dropwise into a three-necked flask, then continue to react for 18 hours, then add 6.2ml of acetic anhydride and 2.1ml of triethylamine, heat up to 45°C and continue to react for 16 hours, after the reaction is completed, cool to room temperature and discharge in ethanol, filter, wash, repeat 2 ~3 times, and finally placed in a vacuum drying oven at 80°C for 24 hours to obtain a tan hyperbranched polyimide polymer, whose structural formula is as follows:

[0041]

Embodiment 3

[0043]Add 0.4413g (1.5mmol) of 3,3',4,4'--biphenyltetracarboxylic dianhydride (BPDA) and 10ml of N-methylpyrrolidone into a three-necked flask, pass in argon, raise the temperature to 30°C, and Triamine Monomer N 2 -(6'-amino-[2,2'-binaphthalen]-7-yl)-N 2 -(5-aminothiophen-2-yl)thiophene-2,5-diamine 0.4786g (1mmol) dissolved in 8ml of N-methylpyrrolidone was evenly added dropwise into the three-necked flask with a constant pressure dropping funnel for 1-2 hours, and then continued the reaction 12h, then add 12ml acetic anhydride and 3ml triethylamine, raise the temperature to 45°C and continue the reaction for 22h, after the reaction is completed, cool to room temperature and discharge the material in ethanol, filter, wash, repeat 2-3 times, and finally place it at 80°C for vacuum drying Dry 24h in the box, obtain the hyperbranched polyimide polymer of tan, and its structural formula is as follows:

[0044]

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Abstract

The invention discloses naphthalene structure-containing high heat-resistant hyperbranched polyimide as well as a preparation method and application thereof. A hyperbranched polyimide material is prepared through imidization by taking triamine containing a naphthalene ring structure and various tetracid dianhydride as raw materials. The hyperbranched polyimide has higher glass-transition temperature, higher thermal stability, lower thermal expansion coefficient and good solubleness. A synthetic method disclosed by the invention is simple in technology and is diversified, so that the syntheticmethod is suitable for industrial production. The hyperbranched polyimide disclosed by the invention has a better application prospect in the field of high temperature resistance and material fields of photosensitive materials, optical waveguide materials, gas permeation and separation films and the like.

Description

technical field [0001] The invention relates to the field of material science, in particular to a high heat-resistant hyperbranched polyimide containing a naphthalene structure and a preparation method thereof. technical background [0002] Polyimide refers to a class of polymers containing imide rings on the main chain. According to the different molecular structures, it can be divided into aromatic polyimide and aliphatic polyimide. Among them, aromatic polyimide has been widely used in many high-tech fields due to its low dielectric properties, high mechanical properties, easy preparation, and especially high thermal stability. [0003] However, in the actual application process, polyimide materials must have special properties and functions that can meet special application purposes on the basis of existing excellent comprehensive properties; for example, as VLSI and microelectronic packaging materials, polyimide In addition to the high heat resistance stability, high ...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08L79/08C08J5/18
CPCC08G73/1003C08G73/1039C08G73/1064C08G73/1067C08G73/1075C08J5/18C08J2379/08
Inventor 谭井华刘亦武黄杰喻仕琦
Owner HUNAN UNIV OF TECH
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