Polyarylketone imidazole and its preparation method

A technology for polyarylketimidazole and bisbenzimidazole is applied in the field of polyarylketimidazole and its preparation, and can solve the problems of harsh operating conditions, complex synthesis process routes, serious environmental pollution and the like, and achieves low preparation cost and simple operation process. Effect

Inactive Publication Date: 2011-12-28
LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the current domestic situation, the tetraamine monomers for the synthesis of polybenzimidazoles have not yet been commercialized, and the synthesis process route of the monomers is complicated, the yield is low, and the cost is high, which hinders the engineering application process of polybenzimidazoles
Polybenzimidazole has two relatively mature synthesis processes, melt polycondensation and solution polycondensation, but the former has harsh operating conditions and requires complex conditions such as high vacuum; the latter has relatively mild reaction conditions, but consumes a large amount of solvent and causes serious environmental pollution.
The overall material of polybenzimidazole has excellent mechanical properties, but its impact resistance is not strong, and it is difficult to apply to occasions with sharp corners, which limits its further use

Method used

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  • Polyarylketone imidazole and its preparation method
  • Polyarylketone imidazole and its preparation method
  • Polyarylketone imidazole and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 50mL three-necked flask, add 0.01mol terephthalic acid, 0.022 o-phenylenediamine, 2mL polyphosphoric acid and 8mL phosphoric acid, under N 2 Under the protection of , the reaction was stirred at 190 °C for 4 h. After the solution is cooled, pour it into 100 mL of cold distilled water, add 15% NaOH solution dropwise, neutralize it to pH=8, and generate a large amount of light green precipitates. After standing for 6 h, the solution was filtered, washed with water and dried to obtain a solid crude product. Dissolve the crude product in N,N- Dimethylformamide was recrystallized and vacuum dried at 60°C to obtain the bisbenzimidazole intermediate- .

[0026]

[0027] Under a nitrogen atmosphere, the bisbenzimidazole intermediate- 0.01mol, 0.01mol of 4'4-difluorobenzophenone, 0.02mol of anhydrous potassium carbonate, 7mL of sulfolane and 3mL of chlorobenzene. The system was raised from room temperature to 145 °C for 2 h. Then the temperature is raised from ...

Embodiment 2

[0031] In a 50mL three-necked flask, add 0.01mol 4'4 diacid diphenyl ether, 0.022 o-phenylenediamine, 2mL polyphosphoric acid and 8mL phosphoric acid, under N 2 Under the protection of , the reaction was stirred at 190 °C for 4 h. After the solution was cooled, pour it into 100 mL of cold distilled water, add 15% NaOH solution dropwise, and neutralize it to pH=8, resulting in a large amount of green precipitates. After the solution was placed for 6 hours, suction filtration, washing with water, and drying were performed to obtain a solid crude product. The crude product was dissolved in absolute ethanol for recrystallization and vacuum drying at 60 °C to obtain the bisbenzimidazole intermediate- .

[0032]

[0033] Under a nitrogen atmosphere, the bisbenzimidazole intermediate- 0.01mol, 0.01mol of 4'4-difluorobenzophenone, 0.02mol of anhydrous potassium carbonate, 7mL of sulfolane and 3mL of chlorobenzene. The system was raised from room temperature to 145 °C for 2 h...

Embodiment 3

[0037] In a 50mL three-neck flask, add 0.01mol 4'4 diacid benzophenone, 0.022 o-phenylenediamine, 2mL polyphosphoric acid and 8mL phosphoric acid, in N 2 Under the protection of , the reaction was stirred at 190 °C for 4 h. After the solution was cooled, pour it into 100 mL of cold distilled water, add 15% NaOH solution dropwise, and neutralize it to pH=8, resulting in a large amount of green precipitates. After the solution was placed for 6 hours, suction filtration, washing with water, and drying were performed to obtain a solid crude product. Dissolve the crude product in N,N - Dimethylformamide (DMF) was recrystallized and vacuum dried at 60°C to obtain the bisbenzimidazole intermediate - .

[0038]

[0039]

[0040] Under a nitrogen atmosphere, the bisbenzimidazole intermediate- 0.01mol, 0.01mol of 4'4-difluorobenzophenone, 0.02mol of anhydrous potassium carbonate, 7mL of sulfolane and 3mL of chlorobenzene. The system was raised from room temperature to 145 ...

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Abstract

The invention discloses a poly(aryl ketone)imidazole and a preparation method thereof, wherein the poly(aryl ketone)imidazole has a structural general formula shown as below. The invention also relates to a preparation method of the poly(aryl ketone)imidazole. The method comprises the steps that aromatic diacids with different structures and o-phenylenediamine are used as monomers to prepare bis(benzimidazole) intermediates with different structures under catalysis of a polyphosphoric acid and phosphoric acid system; monomers of difluoride aromatic ketone and bis(benzimidazole) intermediates,a solvent of sulfolane and a water-removal additive of chlorobenzene are used to prepare poly(aryl ketone)imidazole under catalysis of anhydrous potassium carbonate. The poly(aryl ketone)imidazole prepared by the invention has high glass-transition temperature, high decomposition temperature, excellent mechanical properties, and is prepared through a simple technical operation at low costs.

Description

technical field [0001] The invention relates to a polyarylketone imidazole and a preparation method thereof, more specifically, the invention relates to a heat-resistant polyarylketone imidazole and a preparation method thereof. Background technique [0002] High-performance polymers are considered to be a valuable class of materials for special purposes. Due to their remarkable physical and chemical properties, they can be used in industries such as automobiles, aircraft, aerospace and pharmaceutical industries. Polybenzimidazole is a high-performance polymer. Since its inception, it has become an irreplaceable special material in high-tech fields such as aerospace and other harsh environments. It has been applied abroad, but its key technology is blocked by foreign countries. Although many research institutions in our country are conducting research in this area, they have not yet launched products for engineering applications. From the domestic situation, the tetraamine ...

Claims

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Application Information

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IPC IPC(8): C08G73/18
Inventor 张林常冠军罗炫林润雄
Owner LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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