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Polyimide resin as well as preparation method and application thereof

A polyimide resin and reaction technology, applied in the field of polyimide resin and its preparation, can solve the problems of low solid content, difficult molding processing, poor fluidity, etc., and achieve high glass transition temperature and good melt fluidity , the effect of low solution viscosity

Active Publication Date: 2012-07-25
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, PETI-5 resin has the disadvantages of high melt viscosity, poor fluidity, and difficulty in molding and processing. It can only be prepared by using high-boiling polar organic solvents (such as NMP or DMAc) to produce polyamide with low solid content and high viscosity. Imide resin precursor resin-polyamic acid solution, which is then impregnated with carbon fiber to make prepreg (tape or cloth)
The disadvantage is that the high-boiling-point polar organic solvent contained in the carbon fiber prepreg is difficult to be completely removed in a timely manner during the molding process of the composite material, resulting in a relatively high void ratio of the carbon fiber composite material, which affects the performance and quality of the composite material
In addition, PETI-5 resin has high melt viscosity and poor fluidity, and the lowest melt viscosity at 370 ° C is > 100 Pa.s, and the processing window is narrow, which makes it difficult to process and form carbon fiber composites (Hou.T.H., B.J.Jensen, et al. al. "Processing and properties of IM7 / PETI composites. "Journal of Composite Materials, 1996, 30(1): 109-122)
As we all know, reducing the melt viscosity of polyimide resin can improve the molding process performance of the resin, but with the decrease of the resin melt viscosity, the mechanical properties of the cured resin, especially the toughness will also be significantly reduced

Method used

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  • Polyimide resin as well as preparation method and application thereof
  • Polyimide resin as well as preparation method and application thereof
  • Polyimide resin as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Add 29.74gs-BPDA (0.1011mol), 35g absolute ethanol, and 7g DMF in a 250ml there-necked flask equipped with a mechanical stirrer, a spherical reflux condenser and a thermometer, and heat to reflux for 6 hours under stirring to obtain light Yellow s-BPDA diacid diethyl ester (s-BPDE) homogeneous solution; attached figure 1 It is the 1HNMR spectrum of s-BPDE. It can be seen that s-BPDA has been esterified to form the corresponding diacid diethyl ester (s-BPDE).

[0036] 2) Add 4.96g (0.02mol) 4-PEPA and 10g of absolute ethanol to a 50ml single-necked bottle equipped with an electromagnetic stirring device and a spherical reflux condenser, and heat, stir and reflux for 2 hours to obtain monoethyl monoformate of 4-PEPA (4-PEPE) homogeneous solution;

[0037] 3) Pour this solution into the solution in step 1), then add 18.90g (0.0944mol) 3,4'-ODA and 4.88g (0.0167mol) 1,3,4-APB, supplement ethanol to the solid content of the solution was 48%, stirred at room temperature ...

Embodiment 2

[0039] 1) Add 29.74gs-BPDA (0.1011mol), 35g of anhydrous methanol, and 7g of DMAc in a 250ml there-necked flask equipped with a mechanical stirrer, a spherical reflux condenser, and a thermometer, and heat to reflux for 4 hours under stirring to obtain light Yellow s-BPDA dioic acid dimethyl ester (s-BPDE) homogeneous solution; 2) Add 4.96g (0.02mol) 4-PEPA, 10g Anhydrous methanol is heated and stirred to reflux for 2 hours to obtain a homogeneous solution of monomethyl monoformate (4-PEPE) of 4-PEPA;

[0040] 3) Pour this solution into the solution in step 1), then add 18.90g (0.0944mol) 3,4'-ODA and 4.88g (0.0167mol) 1,3,4-APB, supplement methanol to the solid content of the solution was 49%, stirred at room temperature for 2 hours to obtain a brown polyimide resin homogeneous solution, and its rotational viscosity at 25° C. was 55-60 mPa.s.

Embodiment 3

[0042] 1) Add 29.74gs-BPDA (0.1011mol), 35g absolute ethanol, and 7g NMP in a 250ml there-necked flask equipped with a mechanical stirrer, a spherical reflux condenser and a thermometer, and heat to reflux for 4.5 hours under stirring to obtain a light Yellow s-BPDA diacid diethyl ester (s-BPDE) homogeneous solution;

[0043] 2) Add 4.96g (0.02mol) 4-PEPA and 10g of absolute ethanol to a 50ml single-necked bottle equipped with an electromagnetic stirring device and a spherical reflux condenser, and heat, stir and reflux for 2 hours to obtain monoethyl monoformate of 4-PEPA (4-PEPE) homogeneous solution;

[0044] 3) Pour this solution into the solution in step 1), then add 18.90g (0.0944mol) 3,4'-ODA and 4.88g (0.0167mol) 1,3,4-APB, supplement ethanol to the solid of the solution The content is 47%, stirring at room temperature for 2 hours to obtain a brown polyimide resin homogeneous solution, and its rotational viscosity at 25° C. is 50-56 mPa.s.

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Abstract

The invention discloses polyimide resin with low melt viscosity and high toughness as well as a preparation method of a composite material of the polyimide resin. The resin is high in solid content, low in solution viscosity and is easy to steep carbon fibers to prepare a high-quality carbon fiber prepreg (a belt or cloth); a melt resin formed by heating and melting the resin has the characteristics of low melt viscosity and wide melting temperature; a resin condensate formed by heating and solidifying is high in toughness and high in Tg (glass-transition temperature). The resin is suitable for steeping reinforced fibers to prepare prepregs, and a carbon fiber reinforced composite material prepared by the autoclave and the hot hubbing forming process is excellent in impact-resistant toughness, comprehensive mechanical property and high-temperature resistant performance.

Description

technical field [0001] The invention relates to a polyimide resin and its preparation method and application. Background technique [0002] Carbon fiber-reinforced polyimide resin-based composite materials are widely used in high-tech fields such as aviation, aerospace, space, and rail transportation due to their excellent properties such as light weight, high temperature resistance, low temperature resistance, high specific strength, and high specific modulus. prospect. In recent years, there have been a large number of research reports on the high temperature resistance and molding processability of polyimide resin matrix composites. Generally speaking, polyimide resin can be divided into two categories: thermoplastic and thermosetting. Although thermoplastic polyimide resin has good impact toughness, it has high melt viscosity and poor fluidity, which makes it difficult to combine with carbon fiber. The disadvantages of preparing carbon fiber / polyimide composite materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L79/08C08L77/10C08L27/18C08K7/06C08K7/14C08K7/10C08K3/04C08K3/30B29C43/00
Inventor 杨士勇刘彪冀棉范琳
Owner INST OF CHEM CHINESE ACAD OF SCI
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