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High-temperature-resistant polyimide composite material as well as preparation method and application thereof

A technology of polyimide and composite materials, which is applied in the field of polyimide composite materials and its preparation, and can solve the problems of cumbersome reaction process and high synthesis cost

Active Publication Date: 2022-04-05
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction process of introducing boron or silicon into the PI system is cumbersome and the synthesis cost is high

Method used

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  • High-temperature-resistant polyimide composite material as well as preparation method and application thereof
  • High-temperature-resistant polyimide composite material as well as preparation method and application thereof
  • High-temperature-resistant polyimide composite material as well as preparation method and application thereof

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preparation example Construction

[0045] The invention provides a kind of preparation method of high temperature resistant polyimide composite material, comprises the following steps:

[0046] The imide oligomer monomer and polyimide prepolymer are sequentially subjected to thermal imidization reaction and curing crosslinking reaction to obtain a high temperature resistant polyimide composite material.

[0047] In the present invention, the reaction temperature of the thermal imidization reaction is 240-260°C, preferably 245-255°C, more preferably 250°C. The reaction time is 1.5-2.5 h, preferably 1.8-2.2 h, more preferably 2 h.

[0048] The reaction temperature of the curing crosslinking reaction is 370-390°C, preferably 375-385°C, more preferably 380°C. The reaction time is 1.5-2.5 h, preferably 1.8-2.2 h, more preferably 2 h.

[0049] The concrete operation steps of described preparation polyimide composite material are:

[0050] Stir and dissolve the imide oligomer monomer with dichloromethane, add it to...

Embodiment 1

[0085] Present embodiment is the preparation of imide oligomer monomer, and the raw material used in present embodiment is 4-nitrophthalonitrile (APN), and concrete operation steps are as follows:

[0086] Weigh 45.13g (200mmol) SnCl in a three-necked flask equipped with mechanical stirring 2` 2H 2 O in a 250mL three-necked flask equipped with mechanical stirring, add 50mL of absolute ethanol and stir to dissolve. After the solution is stirred uniformly, add 8.66g (50mmol) of 4-nitrophthalonitrile, and add slowly in batches to prevent Pour the material, stir at room temperature for 10 minutes, then raise the temperature to 80°C to condense and reflux, react for 3 to 4 hours, and use the TCL method to monitor the reaction degree at all times. After the reaction, cool to room temperature, evaporate most of the ethanol solvent, pour into a 500mL beaker, add 150mL deionized water and 150mL ethyl acetate, add solid NaOH, NaHCO 3 The pH of the solution was adjusted to 9, and the s...

Embodiment 2

[0089] This embodiment is the preparation of imide oligomer monomer, and the raw material used in this embodiment is 4-nitrophthalonitrile, and the specific operation steps are as follows:

[0090] Weigh 45.13g (200mmol) SnCl in a three-necked flask equipped with mechanical stirring 2` 2H 2 O in a 250mL three-necked flask equipped with mechanical stirring, add 50mL of absolute ethanol and stir to dissolve. After the solution is stirred uniformly, add 8.66g (50mmol) of 4-nitrophthalonitrile, and add slowly in batches to prevent Pour the material, stir at room temperature for 10 minutes, then raise the temperature to 80°C to condense and reflux, react for 3 to 4 hours, and use the TCL method to monitor the reaction degree at all times. After the reaction, cool to room temperature, evaporate most of the ethanol solvent, pour into a 500mL beaker, add 150mL deionized water and 150mL ethyl acetate, add solid NaOH, NaHCO 3 The pH of the solution was adjusted to 9, and the solution ...

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Abstract

The invention belongs to the technical field of high polymer materials, and discloses a high-temperature-resistant polyimide composite material as well as a preparation method and application thereof. The preparation method comprises the following steps: sequentially carrying out thermal imidization reaction and curing cross-linking reaction on an imide oligomer monomer and a polyimide prepolymer to obtain the high-temperature-resistant polyimide composite material. According to the method, the nitrile group and phenylacetylene group-containing three-functionality imide oligomer monomer is synthesized and introduced into a polyimide system for blending modification, so that a polyimide composite material with very excellent thermal stability is obtained, and the preparation requirements of high-temperature-resistant structural components in the aerospace field are met more and more.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a high-temperature-resistant polyimide composite material and its preparation method and application. Background technique [0002] In recent years, resin-based composite materials have been widely used in the aerospace field due to their light weight, high strength and excellent corrosion resistance, and their proportion in the manufacture of aircraft, missiles and rockets has increased year by year. In the field of heat-resistant polymers, thermosetting polyimide has very outstanding thermal stability and mechanical properties, and has become the most popular resin matrix in the preparation of high-temperature resistant composite materials. The thermal stability of conventional polyimide is closely related to the structure of the molecular body. The thermal decomposition performance varies greatly with the structure of the main chain. The greater the bond energy of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12
Inventor 金成静陈功
Owner BEIHANG UNIV
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