Thermosetting polyimide resin, prepolymer, preparation method and application thereof

A technology of polyimide resin and prepolymer, applied in the field of preparation, thermosetting polyimide resin and prepolymer containing siloxane structure, which can solve the problem of low glass transition temperature of resin and achieve good melt flow properties, high heat resistance, and high melt stability

Active Publication Date: 2020-09-25
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above-mentioned analysis, the present invention aims to provide a kind of thermosetting polyimide resin, prepolymer, preparation method and application, in order to solve existing polyimide resin prepolymer while satisfying RTM molding process requirement , the problem of low glass transition temperature of the resin after curing

Method used

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  • Thermosetting polyimide resin, prepolymer, preparation method and application thereof
  • Thermosetting polyimide resin, prepolymer, preparation method and application thereof
  • Thermosetting polyimide resin, prepolymer, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Add 14.41g (45.0mmol) of 4,4'-diamino-2,2'-bistrifluoromethyl to a three-necked round-bottomed flask equipped with a mechanical stirring paddle, a water separator, a condenser, a nitrogen inlet and outlet, and a thermometer Biphenyl (TFDB), 3.70g (15.0mmol) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane (SIDA) and 70.8g of N- Methylpyrrolidone (NMP), stirred under the protection of nitrogen until completely dissolved to obtain a homogeneous solution, and then 8.38g (26.0mmol) of 2,3,3',4'-benzophenone tetraacid dianhydride (α- BTDA) and 16.88g (68.0mmol) of 4-phenylethynylphthalic anhydride (PEPA) mixed with 30.4g of N-methylpyrrolidone (NMP) were added to the above-mentioned homogeneous solution, and continued to stir at room temperature for 12 After one hour, a polyamic acid resin solution with a solid content of 30 wt.% was obtained. Add 10.1g of toluene to the above polyamic acid resin solution, heat the reaction system to 180°C and reflux for 10 hours, th...

Embodiment 2

[0066] Add 7.64g (36.0mmol) of 4,4'-diaminobenzophenone (DABP), 5.92g ( 24.0mmol) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane (SIDA) and 70.8g of N,N-dimethylacetamide (DMAc ), stirred under nitrogen protection until completely dissolved to obtain a homogeneous solution, then 11.60g (36.0mmol) of 2,3,3',4'-benzophenonetetraacid dianhydride (α-BTDA) and 11.92g (48.0mmol) of 4-phenylethynylphthalic anhydride (PEPA) and 41.7g of N,N-dimethylacetamide (DMAc) mixed slurry was added to the above-mentioned homogeneous solution, and continued to stir and react at room temperature for 12 hours Finally, a polyamic acid resin solution with a solid content of 40 wt.% was obtained. Add 8.4g of toluene to the above polyamic acid resin solution, raise the temperature of the reaction system to 148°C for reflux reaction for 14 hours, distill the toluene off, stop heating, cool the reaction solution to 80-120°C, pour deionized water and A crude resin product was obtained from a mi...

Embodiment 3

[0069] Add 17.29 g (54 mmol) of 4,4'-diamino-2,2'-bistrifluoromethylbisin into a three-necked round-bottomed flask equipped with a mechanical stirring paddle, a water separator, a condenser, a nitrogen inlet and outlet, and a thermometer. Benzene (TFDB), 1.65g (6mmol) of bis(4-aminophenoxy)dimethylsilane (APDS) and 84.3g of N-methylpyrrolidone (NMP), stirred under nitrogen protection until completely dissolved to obtain a homogeneous phase solution, and then 9.31g (30.0mmol) of 2,3,3',4'-diphenyl ether tetra-acid dianhydride (α-ODPA) and 14.89g (60.0mmol) of 4-phenylethynylphthalic anhydride (PEPA ) and 21.1 g of N-methylpyrrolidone (NMP) mixed slurry was added to the above-mentioned homogeneous solution, continued to stir and react at room temperature for 12 hours to obtain a polyamic acid resin solution with a solid content of 30wt.%. Add 10.1g of toluene to the above polyamic acid resin solution, heat up the reaction system to 178°C and reflux for 12 hours, then distill out...

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Abstract

The invention relates to thermosetting polyimide resin, a prepolymer, a preparation method and an application thereof, belong to the technical field of thermosetting polyimide resin, and solve the problem that the glass-transition temperature of cured resin is relatively low while the existing polyimide resin prepolymer meets the requirements of an RTM (resin transfer molding) process. The polyimide resin prepolymer is prepared from aromatic dianhydride, rigid aromatic diamine, diamine containing a siloxane structure and an end-capping reagent. The preparation method of the thermosetting polyimide resin comprises the following steps: heating and melting the prepolymer; heating to 370-400 DEG C, curing for 1-2 hours, and cooling to obtain cured resin; and treating the cured resin at 400-450DEG C for 1-8 hours to obtain the thermosetting polyimide resin. According to the invention, RTM molding process requirements and high temperature resistance are both considered.

Description

technical field [0001] The invention relates to the technical field of thermosetting polyimide resins, in particular to a thermosetting polyimide resin containing siloxane structure, prepolymer, Preparation method and application. Background technique [0002] Thermosetting polyimide resin has been successfully used as a high temperature resistant matrix resin in the manufacture of aerospace vehicle composite components due to its excellent heat resistance stability, excellent mechanical properties, and good dielectric properties. [0003] However, due to the high melt viscosity of traditional high-temperature-resistant polyimide resins, usually only hot molding or vacuum autoclave processes can be used to form composite parts, which has narrow process windows, low production efficiency, and processing Problems such as high cost have seriously restricted the wide application of polyimide resin-based composite materials. [0004] Resin transfer molding (RTM) molding technol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12C08J5/04C08L79/08
CPCC08G73/125C08J5/042C08J5/043C08J5/046C08J2379/08C08J5/0405
Inventor 范琳许晓洲刘仪莫松何民辉
Owner INST OF CHEM CHINESE ACAD OF SCI
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