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Novel phenylacetylene end capacity capped polyimide prepolymer and preparation method thereof

A technology of polyimide and phenylacetylene, applied in the direction of organic chemistry, can solve the problems of molecular rigidity and high polarity, high molecular binding force, difficult composite materials, high melt viscosity, etc., and achieve wide processing window and high production efficiency. High efficiency and good quality effect

Inactive Publication Date: 2009-05-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the two main types of special engineering plastics are polyarylether ketone and polyimide, which have excellent physical properties such as high temperature resistance and high strength, but the fully aromatic structure characteristics of their molecules also lead to the stiffness and high polarity of their molecules. properties, high intermolecular bonding, resulting in these materials usually exhibit high melt viscosity and poor solubility in common organic solvents, making them manufactured composite materials and adhesives by compression molding, injection molding, etc. often present great difficulties

Method used

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  • Novel phenylacetylene end capacity capped polyimide prepolymer and preparation method thereof
  • Novel phenylacetylene end capacity capped polyimide prepolymer and preparation method thereof
  • Novel phenylacetylene end capacity capped polyimide prepolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Embodiment 1: Preparation trimesoyl chloride

[0069] Add 126.0g (0.6mol) trimellitic acid, 256ml (3.6mol) thionyl chloride in the three-necked flask equipped with stirrer, thermometer, dropping funnel, condenser tube, drying tube, tail gas absorption device as solvent, 2ml

[0070] N, N-dimethylformamide DMF is used as a catalyst, and then 511ml (7.2mol) of thionyl chloride is added dropwise to the reaction bottle. After the dropwise addition is completed and stirred for 1.5h, the temperature is raised to 75°C and slightly refluxed for 10h. Acid gas escapes, ending the reaction. Then the water pump decompressed distillation, and thionyl chloride was removed at 59° C. (nitrogen protection during the vacuum distillation process), and 121.6 g of white crystal trimesoyl chloride was obtained, with a yield of 76.3%.

Embodiment 2

[0071] Example 2: Preparation of Trifluoroketone by Friedel's Acylation

[0072] Add 227ml (2.4mol) of fluorobenzene and 80g (0.6mol) of anhydrous aluminum trichloride in a three-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a condenser tube, a drying tube, and an exhaust gas absorption device, and then slowly Add 26.55 g (0.1 mol) of trimesoyl chloride to prevent the reaction from splashing violently. After the addition, continue to stir for 1 h, then raise the temperature to 83° C. and reflux for 6.5 h, then cool down to room temperature and continue the reaction for 9 h. Slowly add the reaction solution to a mixture of 100ml of concentrated hydrochloric acid and 600ml of ice water to remove excess aluminum trichloride, stir while adding, wash with water to neutrality, and use the azeotropic system of fluorobenzene / water to remove fluorobenzene at 80°C Afterwards, the product was dried to obtain 37 g of a crude product with a yield of 83.3%. Take 3...

Embodiment 3

[0073] Embodiment 3: the preparation of triamine monomer

[0074] Add 5.46g (0.05mol) of m-aminophenol, anhydrous potassium carbonate K 2 CO 3 7.60g (0.055mol), 15ml of toluene, 60ml of N,N-dimethylformamide DMF, stirring at room temperature with nitrogen for 10min, then heating, reflux at 134.5°C until no water drops are brought out, then cool the system to 40°C and add trifluoroketone 4.44g (0.01mol), start heating after passing nitrogen gas for 5 minutes, reflux at 134°C until anhydrous, and then release 15ml of toluene, and remove the water-carrying device. The temperature of the system was raised to 147°C, and the reaction was refluxed for 12 hours. Turn off the heating device and lower the temperature to 40°C. After filtering while it is hot, pour the filtrate into a large amount of water and stir to precipitate a red precipitate. Wash the red precipitate repeatedly with water to obtain the crude product, dry it in vacuum at 40°C, and then recrystallize it with ethano...

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Abstract

The invention belongs to the field of polymer materials, and in particular relates to a performed polyimide polymer of two novel phenylacetylene sealed ends and a preparation method thereof. The preparation method is to use diamine 1, 3-di(3, aminobenzene oxyl-4'-formacyl) benzene and triamine 1, 3, 5-tri(3- aminobenzene oxyl-4'-formacyl) benzene respectively with an end-capping reagent - phenylacetylene anhydride to prepare performed polyimide polymer powder of the phenylacetylene sealed ends by the acetone method, the one-step method and the two-step method. The method for preparing the performed polyimide polymer has the advantages of high yield, good quality, high purity and no necessity of performing recrystallization. The performed polyimide polymer of the phenylacetylene sealed ends can be used for preparing high-performance crosslinking materials and has a wide processing window.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, and in particular relates to two novel phenylacetylene-terminated polyimide prepolymers and a preparation method of the prepolymers. Background technique [0002] With the development of cutting-edge fields such as aerospace, people have put forward higher and higher requirements for composite material matrix resins. Therefore, special engineering plastics with high mechanical strength and heat resistance have been developed since the 1960s. As the two main types of special engineering plastics are polyarylether ketone and polyimide, which have excellent physical properties such as high temperature resistance and high strength, but the fully aromatic structure characteristics of their molecules also lead to the stiffness and high polarity of their molecules. properties, high intermolecular bonding, resulting in these materials usually exhibit high melt viscosity and poor solubility in com...

Claims

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Application Information

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IPC IPC(8): C08G73/12C07D209/48
Inventor 陈春海于晓慧赵晓刚党国栋
Owner JILIN UNIV
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