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High performance and low cost polyimide preformed polymer and preparation method thereof

A polyimide and prepolymer technology, applied in the field of polyimide prepolymer and the preparation of the prepolymer, can solve the problems of poor thermal stability and acid resistance, poor processability, and small dissociation energy , to achieve high thermal performance, reduce melt viscosity, and reduce the effect of intermolecular interaction

Inactive Publication Date: 2009-03-25
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, PMR-15, LARC-160, etc. use cross-linkable curable groups with norbornene as the terminal anhydride. This kind of material still maintains the rigid rod-like structure of polyimide, so it has a high glass transition. temperature (T g ), but the processing performance is poor
In addition, the curing reaction of this type of crosslinking group produces a C-C single bond structure with a small dissociation energy, and during the crosslinking reaction, small molecules are released. Due to the existence of this structure, the resin-based composite material of this type Poor thermal stability and acid resistance, low utilization rate

Method used

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  • High performance and low cost polyimide preformed polymer and preparation method thereof
  • High performance and low cost polyimide preformed polymer and preparation method thereof
  • High performance and low cost polyimide preformed polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add N,N-dimethylacetamide (DMAC, 36.10ml) after vacuum distillation into the reaction flask with electromagnetic stirring, and then add 1,4-(p-aminophenoxy)-2-phenyl Benzene (p-TPEQ, 0.02mol, 7.36g), after the diamine is completely dissolved, add dianhydride (PMDA, 0.01mol, 2.18g), the solid content in the solvent is 30%, under nitrogen protection, react at room temperature for 5 hours Add end-capping agent 4-(2-phenylethynyl)phthalic anhydride (PEPA, 0.02mol, 4.96g), and then react for another 2 hours. Wrap a clean glass plate with fluorine tape, then pour the above synthetic polyamic acid solution directly on the glass plate, place the glass plate in an oven, bake at 80°C for 1 hour, and bake at 100°C for 1 hour , then heat up to 150°C and bake for 1 hour to remove the solvent; then remove the powder from the glass plate, put it into a watch glass, place the watch glass in a vacuum oven at a constant temperature of 200°C for 1 hour, and then raise the temperature to a...

Embodiment 2

[0037] Method is as embodiment 1, pyromellitic anhydride (PMDA) is adjusted to (1.33 * 10 -2 mo, 2.90g), the capping agent PEPA is (1.33×10 -2 mol, 3.29), obtain yellow polyimide prepolymer powder 13.29g, more than 97% of productive rate, the molecular weight of the synthetic prepolymer at this moment is about 2000, and the degree of polymerization of polymer is 2. In this example, diamine: dianhydride: capping agent molar ratio = 3:2:2.

Embodiment 3

[0039] Method is as embodiment 1, pyromellitic anhydride (PMDA) is adjusted to (1.60 * 10 -2 mol, 3.49g), capping agent PEPA (8.00×10 -3 mol, 1.98g), obtain yellow polyimide prepolymer powder 12.48g, more than 97% of productive rate, the molecular weight of the prepolymer synthesized at this moment is about 3200, and the degree of polymerization of polymer is 4. In this example, diamine: dianhydride: capping agent molar ratio = 5:4:2.

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Abstract

The invention pertains to the field of polymer materials, in particular to a polyimide prepolymer with comparatively high vitrification transformation temperature (270 DEG C to 320 DEG C), comparatively high stability of thermal oxidization, comparatively low viscosity and comparatively low cost, and a preparation method of the prepolymer. 1, 4-(para-aminophenoxy)-2-phenylbenzene is firstly added into an organic solvent and completely dissolved, then pyromellitic dianhydride is added into the organic solvent and reacts at room temperature for 3 hours to 10 hours, and then an end capping agent, 4-(2-phenylacetylenel) phthalic anhydride is added and the reaction continues for 1 hour to 3 hours. An obtained polyamide acid solution is put into an oven and the solvent is removed; under the condition of vacuum, the temperature is increased for thermal imidization and an obtained product is crushed to obtain the powdered polyimide prepolymer with a structure formula shown as follows.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a polyimide prepolymer with a higher glass transition temperature (270°C-320°C), higher thermo-oxidative stability, lower viscosity and lower cost and the Preparation method of prepolymer. Background technique: [0002] In the early 1980s, resin-based composite materials have been successfully used in the aerospace field. The thermosetting matrix resin used in these composite materials has low heat resistance, and the general heat-resistant temperature is below 135°C, making it difficult to use at high temperatures. In order to meet the requirements of the development of high-speed aircraft and aerospace fields, many scientists have carried out research on various high-temperature resistant and high-performance polymers such as polyethersulfone, polyetherketone, polyarylether, polyetherimide, polyimide, etc. Research and evaluation, but so far, there are few high-tem...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08G73/12
Inventor 周宏伟金倬敏党国栋陈春海赵晓刚
Owner JILIN UNIV
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