Fluorenyl Cardo type polymide diluting agent and preparing method and application thereof

A polyimide diluent, polyimide technology, applied in the direction of adhesives, organic chemistry, etc., can solve the problem of narrowing the processing window of prepolymers, and it is difficult to meet the requirements of resin transfer molding process, glass transition temperature and melting temperature. It can solve problems such as increased bulk viscosity, and achieve the effects of increasing the use temperature range, high solubility and solution stability, and low glass transition temperature.

Inactive Publication Date: 2016-04-20
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method of introducing a fluorene-based structure through copolymerization greatly increases the glass transition temperature and melt viscosity of the polyimide prepolymer before solidification, which w

Method used

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  • Fluorenyl Cardo type polymide diluting agent and preparing method and application thereof
  • Fluorenyl Cardo type polymide diluting agent and preparing method and application thereof
  • Fluorenyl Cardo type polymide diluting agent and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0034] Example 1

[0035] Under the protection of mechanical stirring and inert gas, weigh out 3.48g (0.01mol) of diamine 9,9-bis(4-aminophenyl)fluorene (BAFL) and the blocking agent 4-phenylethynyl phthalic anhydride (PEPA) 4.96 g (0.02mol) in a three-necked flask, drop 32.32g of the organic solvent DMAc after vacuum distillation, and after reacting at room temperature for 8 hours, add triethylamine (0.03mol, 3.04g) and acetic anhydride (0.03mol, 3.06g), reacted at 40°C for 5 hours, and finally the resulting solution was washed 4 times with excess distilled water until the pH of the filtered water was equal to 5, and the resulting product was placed in It was fully dried and pulverized in a vacuum oven at 120°C to finally obtain a powdered polyimide prepolymer diluent, that is, 7.76 g of a fluorene-based reactive diluent, with a yield of 96%.

[0036] Under the protection of nitrogen, add N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation into a three-necked round bottom...

Example Embodiment

[0038] Example 2

[0039] Under the protection of mechanical stirring and inert gas, weigh out 3.48g (0.01mol) of diamine 9,9-bis(4-aminophenyl)fluorene (BAFL) and the blocking agent 4-phenylethynyl phthalic anhydride (PEPA) 4.96 g (0.02mol) in a three-necked flask, drop 32.32g of the organic solvent DMAc after vacuum distillation, after 8 hours of reaction at room temperature, add pyridine (0.02mol, 1.582g) to the resulting polyamic acid solution dropwise ) And acetic anhydride (0.03mol, 3.06g), react at 40°C for 5 hours, and finally wash the resulting solution with excess distilled water 4 times until the pH of the filtered water is equal to 7, and at the same time put the obtained product at 150°C Fully dried and pulverized in a vacuum oven to finally obtain a powdered polyimide prepolymer diluent, that is, 7.76 g of a fluorene-based reactive diluent, with a yield of 96%.

[0040] Under the protection of nitrogen, add N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation ...

Example Embodiment

[0042] Example 3

[0043] Under the protection of mechanical stirring and inert gas, weigh out 3.48g (0.01mol) of diamine 9,9-bis(4-aminophenyl)fluorene (BAFL) and the blocking agent 4-phenylethynyl phthalic anhydride (PEPA) 4.96 g (0.02mol) in a three-necked flask, drop 32.32g of the organic solvent DMAc after vacuum distillation, and after reacting at room temperature for 8 hours, add triethylamine (0.02mol, 2.02g) and acetic anhydride (0.04mol, 4.08g), react at 40℃ for 5 hours, and finally wash the resulting solution with excess distilled water 4 times until the pH value of the filtered water is equal to 7, while placing the resulting product in It was fully dried and pulverized in a vacuum oven at 150°C to finally obtain a powdered polyimide prepolymer diluent, that is, 7.76 g of a fluorene-based reactive diluent, with a yield of 96%.

[0044] Under the protection of nitrogen, add N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation into a three-necked round bottom flas...

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Abstract

The invention relates to a fluorenyl Cardo type polymide diluting agent and a preparing method and application thereof. The structural formula of the diluting agent is shown in the specification. The preparing method comprises the steps that under mechanical stirring and inert gas shielding, BAFL and an end-capping reagent PEPA are dissolved in an organic solvent for a reaction at the room temperature for 2-16 hours, and a polymide acid solution is obtained; then, a dehydrating agent and a dehydrating catalyst are dripped for a reaction at 20-80 DEG C for 3-12 hours, cleaning, filtering, drying and grinding are carried out, and the diluting agent is obtained. The diluting agent is applied to preparation of modified phenylacetylene phthalic terminated polymide resin. By means of the blending modification of the active diluting agent, under the situation that the softening point of a prepolymer is not increased, the glass-transition temperature of the cured polymide resin is increased by 43 DEG C, and the carbon yield in the nitrogen atmosphere at 800 DEG C is increased by 5%; the diluting agent has potential application value in the fields of preparing high-performance advanced composites, high-temperature resistance adhesives and the like as an additive.

Description

technical field [0001] The invention belongs to the technical field of high-performance polymer materials, and in particular relates to a fluorenyl Cardo type polyimide diluent and a preparation method and application thereof. Background technique [0002] Polyimide is a type of polymer containing imide rings in the main chain. It has excellent corrosion resistance, radiation resistance, dielectric properties, insulation, good mechanical properties and high temperature resistance. In the past 30 years, it has received more and more attention and research. As one of the materials with the best comprehensive properties among organic polymer materials, polyimide has been developed into electronic material films, gas separation membranes, plastics, fibers, high temperature resistant adhesives, coatings and advanced composite materials, etc., thus widely It is widely used in various fields of national life and national defense technology such as electronics, chemical industry, m...

Claims

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Application Information

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IPC IPC(8): C08G73/12C07D209/48C09J179/08
CPCC07D209/48C08G73/124C09J179/085
Inventor 胡祖明宇平于俊荣王彦诸静
Owner DONGHUA UNIV
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