Preparation method of polyether-ether-ketone suitable for 3D printing
A polyetheretherketone, 3D printing technology, applied in the direction of additive processing, can solve the problems of low strength, poor stability, poor fluidity, etc., to achieve the effect of less pollutant emission, increased strength, and reduced molecular chain entanglement
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[0015] A method for preparing polyether ether ketone suitable for 3D printing, using sodium carbonate and potassium carbonate as reaction condensation agents, taking hydroquinone and 4,4-difluorobenzophenone as raw materials, and diphenyl sulfone as raw materials Solvent, comprising the following reaction steps:
[0016] (1) Add diphenylsulfone at room temperature, protect with argon, and heat to melt diphenylsulfone at the same time, control the solution temperature at 180-190°C, then add hydroquinone and 4,4-difluorobenzophenone Ketone, and heated to 210 ~ 220 ° C, constant temperature stirring reaction 25 ~ 30min, the mass ratio of hydroquinone, 4,4-difluorobenzophenone, diphenyl sulfone is 1:1:4 ~ 6; Diphenyl sulfone is excessive, the reaction is stable and controllable during the reaction process, which improves the stability of polyether ether ketone;
[0017] (2) Add sodium carbonate and potassium carbonate to the reaction system in step (1), raise the temperature to 2...
Embodiment 1
[0023] (1) Add diphenyl sulfone at room temperature, protect with argon, and heat to melt diphenyl sulfone at the same time, control the solution temperature to 180°C, then add hydroquinone and 4,4-difluorobenzophenone, And heated to 210°C, stirred and reacted at constant temperature for 30 minutes, the mass ratio of hydroquinone, 4,4-difluorobenzophenone, and diphenyl sulfone was 1:1:4;
[0024] (2) Add sodium carbonate and potassium carbonate to the reaction system of step (1), heat up to 230°C, stir and react at a constant temperature for 30min, then heat up to 250°C for 60min, then rapidly heat up to 300°C for constant temperature and use ultrasonic treatment for 30min, then Constant temperature reaction 150min; The frequency of the ultrasonic wave is 22KHz, and the mass ratio of the sodium carbonate, potassium carbonate and hydroquinone is 1:4:14;
[0025] (3) The cooling of the product adopts a segmental cooling method, firstly lowering the temperature to 210°C for 10 mi...
Embodiment 2
[0027] (1) Add diphenyl sulfone at room temperature, protect with argon, and heat to melt diphenyl sulfone at the same time, control the solution temperature to 190°C, then add hydroquinone and 4,4-difluorobenzophenone, And heated to 220°C, stirred and reacted at constant temperature for 25 minutes, the mass ratio of hydroquinone, 4,4-difluorobenzophenone, and diphenyl sulfone was 1:1:6;
[0028] (2) Add sodium carbonate and potassium carbonate to the reaction system of step (1), heat up to 235°C, stir and react at a constant temperature for 25min, then heat up to 260°C for 50min, then rapidly heat up to 320°C for constant temperature and use ultrasonic treatment for 25min, then Constant temperature reaction for 30min; the frequency of the ultrasonic wave is 38KHz, and the mass ratio of sodium carbonate, potassium carbonate and hydroquinone is 1:5:16;
[0029] (3) The cooling of the product adopts a segmented cooling method, firstly lowering the temperature to 220°C for 7 minu...
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