Purification method for preparing polyaryletherketone by electrophilic method
A polyaryletherketone and purification method technology, applied in the field of polyaryletherketone production, can solve problems such as residual metal impurities, and achieve the effects of high processing efficiency and few process steps
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Embodiment 1
[0027] Preparation of polyaryletherketone by electrophilic method:
[0028] Add 270L of dichloromethane solution into the 500L reactor, and then lower the temperature to below -5°C; keep the temperature in the reactor below -5°C, and add 38.98kg of terephthaloyl chloride and 9.74kg of isophthalic dichloride to the reactor respectively Formyl chloride, 41.25kg diphenyl ether; keep the temperature in the reactor not exceeding -5°C, add 35.43kg N,N-dimethylformamide to the reactor; keep the temperature in the reactor not exceeding -5°C, add Add 160kg of aluminum trichloride to the kettle in batches, and continue to stir for 1 to 2 hours after the addition is complete; slowly raise the temperature in the reactor to room temperature, continue stirring until the viscosity no longer changes, stop stirring and aging for 8 hours, and put the reactor inside The colloidal polymer is pulverized with an emulsifier, washed with deionized water, 3-10% hydrochloric acid, and methanol, and the...
Embodiment 2
[0030] The crude polyether ketone ketone prepared in Example 1 is purified by the purification method of the present invention, and the specific steps are as follows:
[0031] In a 1L polytetrafluoroethylene-lined autoclave with mechanical stirring, add 20g of crude polyether ketone ketone, then add 40g of acetylacetone and 200g of xylene, and heat it to 180°C while stirring, After continuing for 30 minutes, gradually lower the temperature, and then wash with hot absolute ethanol for several times, and detect each ethanol washing solution, and filter the obtained polyacetate after no acetylacetone and xylene are detected in the ethanol washing solution. The ether ketone ketone was placed in a vacuum drying oven, and dried under vacuum at 150° C. for 24 hours to obtain purified polyether ketone ketone.
Embodiment 3
[0033] The crude polyether ketone ketone prepared in Example 1 is purified by the purification method of the present invention, and the specific steps are as follows:
[0034] In a 1L polytetrafluoroethylene-lined autoclave with mechanical stirring, add 20g of polyether ketone ketone crude product, and then add 80g of 2-phosphobutane-1,2,4-tricarboxylic acid in water (concentration 50wt%) and 200g deionized water, under stirring, it was heated to 180°C, after 30min, gradually lowered the temperature, then washed several times with hot deionized water, and each deionized water washing solution was Detection, after 2-phosphobutane-1,2,4-tricarboxylic acid is not detected in the washing liquid, filter, put the obtained polyether ketone ketone in a vacuum drying oven, and vacuum dry at 150°C for 24 hours to obtain purified After polyether ketone ketone.
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