A kind of amino-terminated soluble polyaryletherketone and its preparation method and application
A polyaryletherketone and amino-terminated technology, which is applied in the field of amino-terminated soluble polyaryletherketone and its preparation, can solve the problem of inability to improve the adhesion between epoxy resin-based coatings and polyaryletherketone resins or their composite materials , to achieve the effects of solidification, environmental friendliness, cost reduction, and good affinity
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Embodiment 1
[0039] (1) Under the protection of nitrogen atmosphere, add 403g sulfolane (solid content 10wt%), 160mL toluene, 15.9g (150mmol) sodium carbonate, 29.33g (100mmol) difluoromonomer 1 and 11.01g ( 100mmol) Bisphenol monomer 1, heat up to 140°C, azeotropically remove water, reflux for 2h, remove toluene in the reaction system by distillation, heat up to 180-210°C and react for 2h for polymerization, after the polymerization, cool down to 140°C Add 1.08g (5mmol) end-capping agent 1 and react for 2h, pour the reaction product into anhydrous methanol, wash, pulverize and dry to obtain 36.25g polymer 1, then dissolve polymer 1 in 300mL tetrahydrofuran, and wait for the polymer After 1 was completely dissolved, 200 mL of hydrochloric acid solution with pH=0.1 was added to the solution, and after reflux for 24 hours, it was washed with ethanol and water and dried to obtain 27.45 g of amino-terminated crystalline polyaryletherketone polymer 2 powder.
[0040] (2) Lay 5.00 g of crystalli...
Embodiment 2
[0044] (1) Under nitrogen atmosphere protection, add 588g sulfolane (solid content 10wt%), 233mL toluene, 21.8g (150mmol) potassium carbonate, 47.25g (100mmol) difluoromonomer 2 and 13.21g ( 120mmol) bisphenol monomer 1, heat up to 140°C, azeotropically remove water, reflux for 2h, remove the toluene in the reaction system by distillation, then raise the temperature to 180-210°C for 3h to polymerize, after the polymerization is completed, cool down to 140°C Add 2.26g (10mmol) end-capping agent 1 and react for 4h, pour the reaction product into anhydrous methanol, wash, pulverize and dry to obtain 52.18g polymer 3, then dissolve polymer 3 in 400mL tetrahydrofuran, and treat the polymer After 3 was completely dissolved, 200 mL of hydrochloric acid solution with pH=0.1 was added to the solution, and after reflux for 24 hours, it was washed with ethanol and water and dried to obtain 41.88 g of amino-terminated crystalline polyaryletherketone polymer 4 powder.
[0045] (2) Lay 5.00...
Embodiment 3
[0048] (1) Under the protection of nitrogen atmosphere, add 670g sulfolane (solid content 10wt%), 233mL toluene, 16.6g (157mmol) sodium carbonate, 2.68g (8mmol) cesium carbonate, 54.86g (100mmol) biscarbonate successively to the polymerization reaction system Fluorine monomer 3 and 11.01g (100mmol) bisphenol monomer 1 were heated up to 140°C, azeotropically removed water, and refluxed for 4h. After removing toluene in the reaction system by distillation, the temperature was raised to 180-210°C for 3h for polymerization. After the polymerization, the temperature was lowered to 140°C and 4.73g (22mmol) of end-capping agent 1 was added to react for 4h, and the reaction product was poured into anhydrous methanol for washing, pulverized and dried to obtain 61.13g of polymer 5, and 1.5g of polymer 5 Dissolve in 15mL tetrahydrofuran, hydrolyze after spreading film by casting method, add 10mL hydrochloric acid solution with pH=0.1, reflux for 24-48h, then wash with ethanol and water an...
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