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Application of thermosetting polyimide in preparation of high-temperature-resistant resin-based composite material

A high-temperature-resistant resin and polyimide technology, which is applied in the field of preparing high-temperature-resistant resin-based composite materials and thermosetting polyimide, can solve the problems of reducing the mechanical properties of materials and high porosity of composite products, and achieve good application scenarios, The effect of high solubility and high heat resistance

Pending Publication Date: 2022-04-19
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This makes the release of small molecular volatiles water or alcohol in the imidization stage of the resin curing process, resulting in high porosity of composite products, which are prone to defects and reduce the mechanical properties of the material.

Method used

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  • Application of thermosetting polyimide in preparation of high-temperature-resistant resin-based composite material
  • Application of thermosetting polyimide in preparation of high-temperature-resistant resin-based composite material
  • Application of thermosetting polyimide in preparation of high-temperature-resistant resin-based composite material

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preparation example Construction

[0035] In some more specific embodiments, the preparation method of described thermosetting polyimide comprises:

[0036] S1. Under a protective atmosphere, react the mixed reaction system comprising fluorene dianhydride monomer, aromatic diamine monomer and organic solvent at 80-100°C for 6-8 hours;

[0037] S2. Add an end-capping agent to the mixed reaction system described in step S1, and continue the reaction for 2 to 4 hours;

[0038] S3. The temperature of the reaction mixture obtained in step S2 is raised to 170-190° C. and the reaction is continued for 4-6 hours to obtain a polyimide resin.

[0039] In some more specific embodiments, the fluorene dianhydride monomer has a structure as shown in formula (II):

[0040]

[0041] In some more specific embodiments, the aromatic diamine monomers include 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl, 4,4'-diaminobiphenyl Ether, 3,4'-diaminodiphenyl ether, 1,3-bis(3-aminophenoxy)benzene, 1,3-bis(4-aminophenoxy)benzene, 4,...

Embodiment 1

[0062] Under the protection of nitrogen, add 3.931g of 4,4'-diaminodiphenyl ether, 6.000g of fluorene dianhydride monomer and 20g of m-cresol into a 100ml reaction flask, react at 90°C for 6h, and then add 3.249g 4-PEPA, while adding 10g of m-cresol to adjust the solid content of the solution to 30wt%, and continue the reaction for 3h; then under the protection of nitrogen, the reaction system was heated to 185°C for 5h, and the reaction system was cooled to room temperature and then poured into ethanol , filtered, washed, and dried at 250° C. for 2 h to obtain the polyimide shown in formula (i).

[0063]

[0064] Performance characterization: the dissolved solid content of the polyimide prepared in this embodiment can reach 30% in polar aprotic solvent, its 13 CNMR spectrum such as figure 1 As shown, the FT-IR spectrum is shown as figure 2 As shown, the rheological curve is shown as image 3 As shown, the cured product DMA curve of polyimide is as follows Figure 4 As...

Embodiment 2

[0066] Under the protection of nitrogen, 5.210g of 2,2'-bismethyl-4,4'-diaminobiphenyl, 5.000g of fluorene dianhydride monomer and 40g of m-cresol were added to a 100ml reaction flask, at 100 ℃ for 8 hours, then add 6.769g of 4-PEPA, and at the same time add 10g m-cresol to adjust the solid content of the solution to 25wt%, and continue the reaction for 2 hours; then, under the protection of nitrogen, the reaction system is heated to 190 ℃ for 6 hours, and the reaction system After cooling to room temperature, pour it into ethanol, filter, wash, and dry at 260° C. for 3 hours to obtain the polyimide shown in formula (ii).

[0067] The polyimide prepared in this example has a dissolved solid content of up to 30% in a polar aprotic solvent, a minimum melt viscosity of 31Pa·s, a cured product glass transition temperature of 451°C, and a thermal weight loss of 5% in air The temperature is 556°C.

[0068]

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Abstract

The invention discloses application of thermosetting polyimide in preparation of a high-temperature-resistant resin-based composite material. The preparation method of the thermosetting polyimide comprises the following steps: S1, in a protective atmosphere, reacting a mixed reaction system containing a fluorene dianhydride monomer, an aromatic diamine monomer and an organic solvent at 80-100 DEG C for 6-8 hours; s2, adding an end-capping reagent into the mixed reaction system in the step S1, and continuously reacting for 2-4 hours; and S3, heating the reaction mixture obtained in the step S2 to 170-190 DEG C, and continuously reacting for 4-6 hours to obtain the polyimide resin. According to the thermosetting polyimide resin provided by the invention, fluorene dianhydride and aromatic diamine monomers are adopted in a molecular main chain, so that polyimide has the characteristics of good solubility, high heat resistance and the like, and the technical problems of poor solubility and low heat resistance of matrix resin faced by an existing thermosetting polyimide composite material are solved.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to the use of a thermosetting polyimide in preparing a high-temperature-resistant resin-based composite material. Background technique [0002] As a class of high-performance polymers, thermosetting polyimides have attracted more and more attention because of their excellent heat resistance and dielectric properties, diverse synthesis routes and processing routes. In recent years, they have been widely used as matrix resins for composite materials. In aviation, aerospace and other fields. [0003] The traditional polyimide does not have the solubility required by the process because its imidized form does not have the solubility required by the process. The preparation of its composite material is completed by fiber impregnation with amic acid or PMR type (monomer reactant polymerization) resin solution route. This causes the release of small molecule volatile...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC08G73/1039C08G73/1067C08G73/1071
Inventor 孟祥胜阎敬灵王震王献伟蔡牧航
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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