Polyether-ether-ketone capable of being cured as well as preparation method and application thereof
A curing product and polymerization reaction technology, applied in the field of polyetheretherketone manufacturing, can solve problems affecting the performance of polyetheretherketone
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[0111] (1) The preparation method of brominated hydroquinone is characterized in that, in reaction device, add hydroquinone, hydrogen bromide and cuprous sulfate as catalyst, after 3~24 hours of heating reaction at 50~100 ℃, ethyl acetate The crude product was obtained after ester extraction, washing with water and drying to remove the organic solvent. The crude product was recrystallized from chloroform and dried in vacuo to obtain a white solid product. The molar ratio of the diphenol, hydrogen bromide and cuprous sulfate catalyst is 1~1.8:1~10:1;
[0112] (2) The preparation method of the p-diphenol intermediate of silane protection, it is characterized in that, under inert gas protection, the brominated p-diphenol obtained in step (1) and tert-butyldimethylchlorosilane or trimethylchlorosilane Mix with imidazole in N,N-dimethylformamide, then react at 20-80°C for 5-24 hours. After the reaction, the reaction solution was poured into water and extracted with chloroform. T...
Embodiment 1
[0127] The synthesis of embodiment 1 precursor 2-bromo-1,4-bisphenol
[0128]
[0129] In a 100 ml two-necked flask, add 1,4-hydroquinone (13.3 g, 121 mmol), copper nitrate trihydrate (4.5 g, 21 mmol) and hydrogen bromide (40%, 44 ml, 324 Millimoles). Heated to 80°C, reacted overnight, and air was blown in during the reaction. After cooling to room temperature, an aqueous solution of sodium bisulfite (10%) was added to the reaction mixture, and the aqueous solution was extracted with ethyl acetate. The organic phase was washed with water until neutral, and dried over anhydrous sodium sulfate. After removing the organic solution, the resulting solid was recrystallized with chloroform to finally obtain 14.5 g of a white solid with a yield of 64%. 1 H NMR (400MHz, CHCl 3 ) δ (ppm) 6.98 (d, 1H, ArH), 6.89 (d, 1H, ArH), 6.73 (dd, 1H, ArH), 5.12 (s, 1H, OH), 4.53 (s, 1H, OH).
Embodiment 2
[0130] Synthesis of 2-bromo-1,4-diphenol of embodiment 2 silane protection
[0131]
[0132] Under argon protection, 2-bromo-1,4-diphenol (7.31 g, 38.9 mmol), tert-butyldimethylsilyl chloride (29.3 g, 194 mmol) and imidazole (11.9 g, 175 mmol ) into 250 ml two-neck flasks, and then 100 ml DMF, and stirred overnight at room temperature. The reaction mixture was poured into 100 ml of water, extracted 3 times with dichloromethane, and the organic phases were combined. Wash twice with 5% dilute hydrochloric acid, once with saturated aqueous sodium bicarbonate, then with water until neutral, and dry over anhydrous sodium sulfate. After removing the solvent, the crude product was separated and purified by column chromatography (silica gel, n-hexane as eluent) to obtain 14.8 g of white crystals with a yield of 92.0%. 1 H NMR (400MHz, CDCl 3 )δ(ppm)7.01(d,1H,ArH),6.72(d,1H,ArH),6.64(dd,1H,ArH),1.02(s,9H,CH 3 ),0.96(s,9H,CH 3 ),0.21(s,6H,CH 3 ),0.16(s,6H,CH 3 ).Mass spectrum:...
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