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Low viscosity polyimide copolymerized thermosetting resin and preparation method and application thereof

A polyimide and oligomer technology, which is applied in the field of low-viscosity copolymerization thermosetting polyimide materials and its preparation, can solve the problems that the processing performance has not been improved, and it is difficult to improve heat resistance, so as to reduce viscosity and improve Improvement of fluidity and heat resistance stability

Inactive Publication Date: 2019-03-15
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN201610677926.3 provides a polyimide resin system containing a carborane structure, the glass transition temperature of which can reach above 500°C, but the minimum viscosity of the resin is also above 1000Pa·s, and the processing performance is not good. be improved
[0007] At present, it is difficult for polyimide resin to improve heat resistance while reducing viscosity and improving processing performance, and vice versa

Method used

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  • Low viscosity polyimide copolymerized thermosetting resin and preparation method and application thereof
  • Low viscosity polyimide copolymerized thermosetting resin and preparation method and application thereof
  • Low viscosity polyimide copolymerized thermosetting resin and preparation method and application thereof

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Embodiment 1

[0053] The preparation of embodiment 1 polyimide oligomer PI-2

[0054] (1) Take the raw material ratio a:b:c:d=0.8:3.2:3:2, the specific operation is: add c component 6.9g, d component 3.88g and 50ml solvent absolute ethanol in the three-necked flask , the oil bath was refluxed at 70°C for 3h, the reaction solution changed from turbid to clear, and was left to cool to room temperature.

[0055] (2) 0.55 g of component a and 5.9 g of component b were sequentially added to the above reaction solution, and stirred and reacted at 25° C. for 12 hours to obtain a yellow clear polyamic acid solution (solid content 30±5%). The obtained solution was placed in a vacuum oven to remove the solvent, then placed in a tube furnace at 260° C. for 1.5 h, cooled naturally, and ground to obtain a yellow polyimide prepolymer powder. This prepolymer was named "prepolymer PI-2".

[0056] According to the method similar to Example 1, adjust the dosages of the four components respectively as shown...

Embodiment 2

[0059] The preparation of embodiment 2 thermosetting polyimide materials

[0060] The prepolymer obtained in Example 1 was cured in a vacuum tube furnace according to the following procedures: within 60 minutes, the temperature was raised from room temperature to 320 °C and kept for 10 minutes; within 20 minutes, the temperature was raised to 370 °C and kept for 2 hours, and naturally cooled to obtain the corresponding polyamide Imines PI-2, PI-3, PI-4 and PI-5.

Embodiment 3

[0061] The preparation of embodiment 3 polyimide composite material

[0062] (1) Preparation of carbon fiber prepreg: the polyamic acid ethanol solution (for the polyamic acid mentioned in Example 1) with a solid content of 30% is evenly coated on the T700 carbon fiber unidirectional woven cloth, and placed in a blast Stand in an oven at 40°C for 6 hours to evaporate most of the solvent, and you get it;

[0063] (2) Preparation of composite materials: Cut the prepreg into 7 layers of sheets with a size of 100mm×100mm and spread them in the mold, and then place the mold on a hot press for thermal imidization of the prepolymer and resin curing process, that is Obtain a T700 carbon fiber / polyimide composite laminate with a thickness of 2mm. See the appendix for the specific heating program Figure 7 .

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Abstract

The invention relates to the technical field of high molecular materials, and particularly relates to copolymerized polyimide thermosetting resin comprising a carborane structure and a preparation method and an application thereof. The copolymerized polyimide resin is prepared by thermally cross-linking and solidifying polyimide oligomers represented by a formula I as a raw material. The oligomersintroduce the carborane of a certain composition into a conventional thermosetting polyimide resin system by means of a copolymerization method, so that the conventional thermosetting polyimide resinhas relatively low hot melt viscosity and a higher glass-transition temperature (higher than 500 DEG C) and also has more excellent thermal oxidation resistance and heat stability resistance. Therefore, the thermosetting resin has the extremely low hot melt viscosity. The resin is more easily prepared into a composite material part of a complex structure through a conventional processing technology, can improve the thermal oxidation resistance of the material to a great extent, and has very high application value and innovation to prepare a light high strength high-temperature-resistant easily processed polyimide composite material for a structural material in the aerospace field.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a carborane-containing low-viscosity copolymerization type thermosetting polyimide material, a preparation method and an application. Background technique [0002] Since the advent of thermosetting polyimide resin, it has been known for its heat resistance and thermal oxidation resistance. From the perspective of molecular structure, polyimide has good heat resistance and thermal oxidation resistance, mainly due to the large number of benzene ring rigid groups in the macromolecular chain, which improves the stability of the macromolecular chain segment. The introduction of a large number of rigid benzene rings will bring another problem, that is, the resin viscosity is high when the composite material is prepared, the processability is poor, and the molding process requires high requirements. One of the most representative thermosetting polyimides of this t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12C08L79/08C08K7/06C08J5/24
CPCC08G73/126C08J5/24C08J2379/08C08K7/06
Inventor 邹宇凯武元娥陈功杨继萍
Owner BEIHANG UNIV
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