A kind of thermosetting polyimide prepolymer and its preparation method and application

A polyimide and prepolymer technology, applied in the field of high-performance polymer materials, can solve problems such as inability to adapt to processing equipment, limit development and application, and narrow melt processing window, so as to improve solution stability and improve melt processing Window, Ease of Melt Processing

Active Publication Date: 2020-08-25
常州杰铭新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the 1970s, in order to obtain high-performance composite materials with good processability, the National Aeronautics and Space Administration (NASA) researched and developed the in-situ polymerization (PMR) process of monomer reactants, and synthesized and prepared the first generation of resin PMR-15. It has the advantages of easy processing, excellent mechanical properties, and good thermal-oxidative stability. It has been the preferred matrix resin for aero-engines for a long time, but it also has some defects, including high monomer toxicity, and the preparation of composite materials is easy. Cracks and small molecule solvents will be released during processing, these defects will limit its further development and application
Later, ethynyl-terminated thermosetting polyimides received a lot of attention. This type of polymer maintains the thermal stability of the material, but the melt processing window is too narrow, making it difficult to melt process, let alone adapt to advanced processing. equipment

Method used

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  • A kind of thermosetting polyimide prepolymer and its preparation method and application
  • A kind of thermosetting polyimide prepolymer and its preparation method and application
  • A kind of thermosetting polyimide prepolymer and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0031]Under nitrogen protection, add N-methylpyrrolidone (NMP, 20g) after vacuum distillation in a three-necked round-bottomed flask with mechanical stirring, then add 4-phenoxy m-phenylenediamine (0.04mol , 8g), after it was completely dissolved, accurately weighed 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (0.02mol, 6.2g) and 20gNMP, and the reaction temperature was reacted at room temperature for 6 hours Add end-capping agent 4-phenylacetylene phthalic anhydride (0.04mol, 9.92g) and NMP solvent, control the solid content of solution at 30wt%, continue to stir and react for 16 hours, then add triethylamine dropwise in the polyamic acid solution that generates Amine (0.12mol, 12.12g) and acetic anhydride (0.12mol, 12.24g) were reacted at room temperature for 6 hours, and finally the resulting solution was washed with 1000mL of distilled water for 3 times until the pH value of the filtered water was approximately equal to 7, while The obtained product was fully dried...

Embodiment 2

[0033] Under nitrogen protection, add N-methylpyrrolidone (NMP, 35g) after vacuum distillation in a three-necked round bottom flask with mechanical stirring, then add 4-phenoxy m-phenylenediamine (0.05mol , 10g), after it was completely dissolved, accurately weighed 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (0.04mol, 12.4g) and 35gNMP, and the reaction temperature was reacted at room temperature for 6 hours Add end-capping agent 4-phenylacetylene phthalic anhydride (0.02mol, 4.96g) and NMP solvent, control the solid content of solution at 30wt%, continue to stir and react for 16 hours, then add triethylamine dropwise in the polyamic acid solution that generates Amine (0.15mol, 15.15g) and acetic anhydride (0.15mol, 15.30g) were reacted at room temperature for 6 hours, and finally the resulting solution was washed with 1000mL of distilled water for 3 times until the pH value of the filtered water was approximately equal to 7, while The obtained product was fully drie...

Embodiment 3

[0035] Under the protection of nitrogen, in a three-necked round bottom flask with mechanical stirring, add N-methylpyrrolidone (NMP, 5g) after vacuum distillation, then add 4-phenoxy m-phenylenediamine (0.01mol , 2g), after it was completely dissolved, accurately weighed 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (0.009mol, 2.79g) and 5gNMP, and the reaction temperature was reacted at room temperature for 4 hours Add the end-capping agent 4-phenylacetylene phthalic anhydride (0.002mol, 0.496g) and the remaining NMP solvent, control the solid content of the solution at 20wt%, continue to stir and react for 20 hours, and then add it dropwise in the polyamic acid solution generated Triethylamine (0.02mol, 2.02g) and acetic anhydride (0.02mol, 2.04g) were reacted at room temperature for 12 hours, and finally the resulting solution was washed 4 times with 100mL of distilled water until the pH value of the filtered water was approximately equal to 7 At the same time, the ...

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Abstract

The invention relates to a thermosetting polyimide prepolymer and a preparation method and application thereof. The preparation method comprises stirring meta-diamine having a bulky aromatic epoxy side group, 2, 3, 3', 4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA) and a blocking agent 4-phenylethynylphthalic anhydride as monomers at the room temperature for a reaction to produce a polyamide acid prepolymer solution, carrying out catalytic dehydration to obtain a polyimide prepolymer solution, and carrying out washing, drying and crushing to obtain polyimide prepolymer powder. The preparation method has a yield of 95% or more. The thermosetting polyimide prepolymer has very high solubility, melt flowability and a high melting processing window and has a high glass transition temperature after curing. The thermosetting polyimide prepolymer has a certain application value in the preparation of high-performance advanced composite materials, high temperature resistant adhesives andhigh temperature-resistant bearing parts.

Description

technical field [0001] The invention belongs to the technical field of high-performance polymer materials, and in particular relates to a thermosetting polyimide prepolymer and its preparation method and application. Background technique [0002] As an important member of the high-performance polymer family, polyimide (PI) can be made into thin films due to its very high thermal oxygen stability, good mechanical properties, excellent dimensional stability and solvent corrosion resistance. , fibers, adhesives, engineering plastics, coatings and advanced composite materials and other products, which have irreplaceable applications for other materials in the fields of electronic appliances, engineering plastics, automobiles, aerospace and advanced resin-based composite materials. Polyimide can be divided into thermoplastic polyimide and thermosetting polyimide according to different processing techniques. Thermoplastic PI is generally a polymer with a linear structure and high...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10
CPCC08G73/1007C08G73/1071
Inventor 宇平王巍胡一鸣
Owner 常州杰铭新材料科技有限公司
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