Preparation method of thermosetting polyimide

A polyimide and thermosetting technology, applied in the field of preparation of thermosetting polyimide, can solve the problems of low mechanical strength, low transition temperature, and the failure of reprocessing and recycling of high-performance polymers

Active Publication Date: 2019-06-28
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0004] However, the above-mentioned related studies are all based on elastomers with low transition temperature and low mechanical strength, and reprocessing and recycling of high-performance polymers such as polyimide have not yet been realized.

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  • Preparation method of thermosetting polyimide
  • Preparation method of thermosetting polyimide
  • Preparation method of thermosetting polyimide

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preparation example Construction

[0025] The invention provides a kind of preparation method of thermosetting polyimide, comprises the following steps:

[0026] 1) Diamine, dianhydride and organic solvent are mixed, carry out polycondensation reaction, obtain the polyamic acid solution of diamine termination;

[0027] 2) mixing the diamine-terminated polyamic acid solution with toluene to carry out an imidization reaction to obtain a polyimide oligomer;

[0028] 3) Mixing the polyimide oligomer, trimesaldehyde and an organic solvent for cross-linking and condensation reaction to obtain a thermosetting polyimide.

[0029] The invention mixes diamine, dianhydride and organic solvent to carry out polycondensation reaction to obtain diamine-terminated polyamic acid solution. In the present invention, the diamine is preferably 3,3'-diaminodiphenyl ether, 4,4'-diaminodiphenyl sulfone, 4,4'-diaminodiphenyl ether, 2,2-bis[ One of (4-aminophenoxy)phenyl]propane, 4,4'-diaminodiphenylmethane, 1,4-butanediamine and 1,4-...

Embodiment 1

[0042] Dissolve 4,4'-diaminodiphenyl ether (10 mmol) in N-methyl-2-pyrrolidone, stir at room temperature under a dry nitrogen atmosphere until completely dissolved, then add bisphenol A diether dianhydride ( 5mmol), stir 12h under nitrogen atmosphere, ice-water bath condition, carry out polycondensation reaction, obtain the polyamic acid solution of diamine termination; In described polyamic acid solution, add toluene (toluene and N-methyl-2-pyrrolidone Volume ratio 1:10), reflux at 250°C for 5h to carry out imidization reaction; after cooling to room temperature, pour the resulting reaction liquid into methanol to precipitate solids, vacuum filter the resulting system, wash with toluene three times, and Vacuum drying at 80°C to obtain a polyimide oligomer;

[0043] Add N-methyl-2-pyrrolidone (10mL) in the polyimide oligomer (1mmol), stir constantly until completely dissolving to obtain a transparent solution, add trimesaldehyde-containing N to the solution. ,N-Dimethylformam...

Embodiment 2

[0049] Dissolve 4,4'-diaminodiphenyl ether (10 mmol) in N-methyl-2-pyrrolidone, stir at room temperature under a dry nitrogen atmosphere until completely dissolved, then add 4,4'-(hexafluoroiso Propylene) diphthalic anhydride (5mmol), stir 10h under nitrogen atmosphere, ice-water bath condition, carry out polycondensation reaction, obtain the polyamic acid solution of diamine termination; In described polyamic acid solution, add toluene (toluene and N-formaldehyde Base-2-pyrrolidone volume ratio 1:10), reflux at 220°C for 8h to carry out imidization reaction; after cooling to room temperature, pour the reaction liquid into ethanol to precipitate solids, vacuum filter the obtained system, and use Washing with toluene three times and drying in vacuum at 100°C to obtain a polyimide oligomer;

[0050] Add N-methyl-2-pyrrolidone (10mL) in the polyimide oligomer (1mmol), stir constantly until completely dissolving to obtain a transparent solution, add trimesaldehyde-containing N to ...

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Abstract

The invention belongs to the technical field of macromolecular materials, and particularly relates to a preparation method of recyclable thermosetting polyimide. The preparation method of recyclable thermosetting polyimide includes the steps that firstly, an amine end capping method is adopted to obtain polyimide oligomers with active reaction amino groups, and then a cross-linking agent containing multiple aldehyde groups is adopted to conduct cross-linking condensation to obtain thermosetting polyimide. Thermosetting polyimide prepared through the preparation method maintains excellent performance of polyimide and can be recycled and reprocessed; not only can thermosetting polyimide prepared through the preparation method be decomposed and recycled, but also recycled monomers still can be recycled again, a material obtained after the recycled monomers are polymerized again still has the same mechanical performance as the raw material, and the preparation method is mainly applied to recycling and the like of composite materials; the vitrification transformation temperature of thermosetting polyimide prepared through the preparation method is greater than 200 DEG C, and thermosetting polyimide can be applied to severe environments such as high-temperature environments.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of thermosetting polyimide. Background technique [0002] With the lightweight and intelligentization of national defense equipment, thermosetting polymers and their composite materials are widely used in aerospace and national defense construction due to their excellent comprehensive properties, playing an irreplaceable role. However, it is difficult for thermosetting polymers to repair themselves after damage, which seriously limits their service life, and these thermosetting polymer wastes are generally disposed of by means of landfill or incineration, which cannot be reprocessed and recycled, resulting in serious waste of resources and environmental pollution. pollute. Therefore, it is of great significance to overcome the shortcomings of traditional thermosetting polymers and explore new reprocessed and recycled materials for the r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08G73/12
Inventor 杨增辉王齐华张新瑞张耀明陶立明王廷梅
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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