Methoxy polyaromatic ether ketone resin and preparation method thereof
A technology of methoxy polyarylether and methoxy aryl ether, which is applied in the field of methoxy polyarylether ketone resin and its preparation, can solve the problems of reducing production cost and achieve low production cost, good heat resistance, The effect of mild reaction conditions
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Embodiment 1
[0035] Preparation of Methoxyaryl Ether Monomer
[0036] Add 0.22mol o-methoxyphenol, 50ml N-methylpyrrolidone, 0.22mol sodium hydroxide, and 80ml toluene to a three-necked flask equipped with a mechanical stirrer, reflux dehydration device, and nitrogen protection, and the mixture is heated at 140°C in an oil bath. Heating under reflux for dehydration, until the reaction is complete to remove the water, the temperature of the oil bath is raised to 160°C to distill the toluene. Cool slightly, add 0.1mol of 4,4-dichlorodiphenyl sulfone, and adjust the oil bath temperature to 190-200°C, and react for 5-6h. After the reaction was completed, the reactant was poured into water to precipitate a precipitate, filtered with suction, washed once with dilute sodium hydroxide solution, and washed once with cold and hot water to obtain a white solid with a yield of 94%. The prepared monomer was recrystallized twice, dried and measured for melting point. The melting point of the product i...
Embodiment 2
[0039] Add 0.22mol o-methoxyphenol, 50ml sulfolane, 0.22mol potassium carbonate, and 80ml toluene to a three-necked flask equipped with a mechanical stirrer, reflux dehydration device, and nitrogen protection, and heat the mixture under reflux dehydration at a temperature of 150°C in an oil bath. After the reaction was completed, the water was removed, and the temperature of the oil bath was raised to 160°C to distill off the toluene. Cool slightly, add 0.1mol of 4,4-dichlorodiphenyl sulfone, and adjust the temperature of the oil bath to 200°C, and react for 5-6h. After the reaction was completed, the reactant was poured into water to precipitate a precipitate, filtered with suction, washed once with dilute sodium hydroxide solution, and washed once with cold and hot water to obtain a white solid with a yield of 95%. The prepared monomer was recrystallized twice, dried and measured for melting point. The melting point of the product is 241-242°C.
Embodiment 3
[0041]Add 0.22mol o-methoxyphenol, 50ml N-methylpyrrolidone, 0.22mol potassium hydroxide, and 80ml toluene to a three-necked flask equipped with a mechanical stirrer, reflux dehydration device, and nitrogen protection, and the mixture is heated at 140°C in an oil bath. Heating under reflux for dehydration, until the reaction is complete to remove the water, the temperature of the oil bath is raised to 160°C to distill the toluene. Cool slightly, add 0.1mol of 4,4'-difluorobenzophenone, and adjust the oil bath temperature to 180-190°C, and react for 5-6h. After the reaction was completed, the reactant was poured into water to precipitate a precipitate, filtered with suction, washed once with dilute sodium hydroxide solution, and washed once with cold and hot water to obtain a white solid with a yield of 96%. The prepared monomer was recrystallized twice, dried and measured for melting point. The melting point of the product is 133-134°C.
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