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High-fluidity wide-processing-widow polyimide pre-polymer and preparation method thereof

A polyimide and processing window technology is applied in the field of thermosetting prepolymer materials and their preparation, which can solve the problems of high melt viscosity and low glass transition temperature, and achieve low melt viscosity and lower glass transition temperature. , the effect of reducing production costs

Active Publication Date: 2015-04-22
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the 1980s, research institutions represented by NASA in the United States developed more than 100 kinds of phenylacetylene-terminated polyimide (PETI) series prepolymers, among which PETI-5 has good mechanical properties and processability. A representative variety, but its glass transition temperature after crosslinking is relatively low at only 270°C, and its melt viscosity is relatively high, with a minimum melt viscosity of 60000Pa·s (371°C)

Method used

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  • High-fluidity wide-processing-widow polyimide pre-polymer and preparation method thereof
  • High-fluidity wide-processing-widow polyimide pre-polymer and preparation method thereof
  • High-fluidity wide-processing-widow polyimide pre-polymer and preparation method thereof

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Embodiment 1

[0032] Under nitrogen protection, N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation was added in a three-necked round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether ( 3,4'-ODA, 0.04mol, 8g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.02mol, 6.2g) , add DMAc again, control reaction concentration (the sum of diamine and dianhydride is solute) at 30%, reaction temperature adds end-capping agent phenylacetylene phthalic anhydride (PEPA, 0.04mol, 9.92g) after reacting at room temperature for 4 hours, Continue to react for 2 hours, then add triethylamine (0.08mol, 8.08g) and acetic anhydride (0.12mol, 12.24g) dropwise in the polyamic acid solution generated, react at room temperature for 5 hours, and finally the solution obtained Rinse twice with 1000mL of distilled water until the pH value of the filtered water is approximately equal to 7. At the same time, place the obtain...

Embodiment 2

[0034] Under nitrogen protection, N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation was added in a three-necked round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether ( 3,4'-ODA, 0.04mol, 8g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.027mol, 8.27g) , add DMAc again, control reaction concentration (the sum of diamine and dianhydride is solute) at 30%, reaction temperature adds end-capping agent phenylacetylene phthalic anhydride (PEPA, 0.02mol, 6.61g) after reacting at room temperature for 4 hours, Continue to react for 2 hours, then add triethylamine (0.08mol, 8.08g) and acetic anhydride (0.12mol, 12.24g) dropwise in the polyamic acid solution generated, react at room temperature for 5 hours, and finally the solution obtained Rinse twice with 1000mL of distilled water until the pH value of the filtered water is approximately equal to 7. At the same time, place the obta...

Embodiment 3

[0040] Under nitrogen protection, N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation was added in a three-necked round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether ( 3,4'-ODA, 0.04mol, 8g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.032mol, 9.2g) , add DMAc again, control reaction concentration (the sum of diamine and dianhydride is solute) at 30%, reaction temperature adds end-capping agent phenylacetylene phthalic anhydride (PEPA, 0.016mol, 3.968g) after reacting at room temperature for 4 hours, Continue to react for 2 hours, then add triethylamine (0.08mol, 8.08g) and acetic anhydride (0.12mol, 12.24g) dropwise in the polyamic acid solution generated, react at room temperature for 5 hours, and finally the solution obtained Rinse twice with 1000mL of distilled water until the pH value of the filtered water is approximately equal to 7. At the same time, place the obt...

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Abstract

The invention relates to a high-fluidity wide-processing-widow polyimide pre-polymer and a preparation method thereof. A structural formula is shown in the description, wherein n is 1-20 and is an integer. The preparation method comprises the steps of dissolving 3,4'-diaminodiphenyl ether 3,4'-ODA in an organic solvent under the nitrogen protection condition, adding 2,3,3',4'-tetracarboxydiphthalic ether dianhydride a-ODPA after complete dissolution, meanwhile adding the organic solvent to enable the solid content of a solution to be 10%-40%, adding an end-capping reagent during reaction at the room temperature to continue to perform reaction, dropwise adding a dehydrating agent to perform reaction, washing, drying and smashing. The pre-polymer can be formed through compression molding, is well applicable to a resin transfer forming process and has potential application value on the aspect of preparation of high-performance composite materials, high-temperature-resisting adhesives and the like.

Description

technical field [0001] The invention belongs to the field of thermosetting prepolymer materials and preparation thereof, in particular to a polyimide prepolymer with high fluidity and wide processing window and a preparation method thereof. Background technique [0002] In the past 30 years, polyimide has played a very important role in new materials and high-tech fields due to its very high thermal oxygen stability, excellent chemical properties and excellent mechanical properties. It has been prepared into a variety of products, including films, fibers, adhesives, engineering plastics, coatings and advanced composite materials. [0003] In order to solve the processing problems of low solubility and high melt viscosity of high-performance polymers, and to meet the demand for new materials in the aerospace and microelectronics fields, the research and development of polyimide prepolymers containing reactive groups has attracted scientists. Widespread concern. This kind of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12C07D209/48
Inventor 胡祖明宇平王彦诸静于俊荣
Owner DONGHUA UNIV
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