Full-biphenyl polyaryletherketone precursor as well as preparation method and application thereof
A technology of polyaryletherketone and all-biphenyl type, which is applied in the field of all-biphenyl type polyaryletherketone precursor and its preparation, can solve the problems of high melting point and high molecular weight, increase the molecular weight of the polymer, and reduce the energy consumption of polymerization , Reduce the effect of side effects and gel content
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[0035] Example 1:
[0036] Under the protection of a nitrogen atmosphere, 4248 g of cyclobutolane (solid content 10 wt%), 1010 ml toluene, 207 g of potassium carbonate, 286 g of dual fluoride monomer 1 and 186 g of biphenol were sequentially added to the polymerization reaction system, and the heated to 140 ° C, and Water, refluxing 2 h, by distillation, toluene in the reaction system, warmed to 190-210 ° C for 6 h, pour the reaction product into anhydrous methanol, wash and dried and dried to obtain a precursor, then dissolved in 4320 ml In THF, it was dissolved in a solution to the solution, and 540 ml of pH = 0.1 hydrochloric acid solution was added to the solution. After refluxing for 24 h, then the crystalline allophenyl polyether ether ketone (PEDEK) was obtained, and the crystalline allxes were washed and dried. PEDEK's characteristic viscosity is 2.09dl / g, T m It was 416.8 ° C.
Example Embodiment
[0037] Example 2:
[0038] Under the protection of a nitrogen atmosphere, 976 g of diphenyl sulfone (solid content of 30 wt%), 419 ml of xylene, 158.8 g of sodium carbonate, 294 g of double fluoride monomer 2 and 204.6 g of biphenol, heated to 180 EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc. The precursor was dissolved in 4586 ml of chloroform. After the precursor dissolution, 179 g of dimethyl sulfoxide and 211 g 2-iodo-2-methylpropane were sequentially added, and the reaction product was poured into anhydrous water after 70 ° C for 48 h. In methanol, then washed with anhydrous methanol and dried to obtain a crystalline all-stranded benzene polyether ether ketone (PEDEK), PEDEK's characteristic viscosity is 2.09 dl / g, T m It is 416.8 ° C.
Example Embodiment
[0039] Example 3:
[0040] Under the protection of a nitrogen atmosphere, 4575 g of cyclobutolane (solid content 10 wt%), 1088 ml of toluene, 196.7 g of potassium carbonate, 24.4 g of cesium carbonate, 322.3 g of dual fluoride 3 and 186 g of bicyphhenol, heating To 140 ° C, the water was concentrated, refluxed for 2 h, and the toluene in the reaction system was removed, and the reaction product was warmed to 190 ° C to 210 ° C for 6 h, and the reaction product was poured into anhydrous methanol, pulverized and dried. Further, the precursor is dissolved in 4683 ml DMF. When the protrusion body is dissolved, 585 ml of pH = 0.1 mesylate solution is added to the solution. After refluxing 24 h, then washed with ethanol and water, and the crystallinity is obtained. Benzene polyether ether ketone (PEDEK), PEDEK's characteristic viscosity is 2.09 dl / g, T m It is 416.8 ° C.
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