Benzoxazine-terminated fluorenyl polyether ketone ketone thermoplastic resin and preparation method thereof
A fluorene-based polyetherketone ketone and thermoplastic resin technology, which is applied in the field of thermoplastic resin preparation, can solve problems such as brittleness of benzoxazine, and achieve the effects of improved mechanical properties and good thermal properties
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Embodiment 1
[0015] Add 5.72g of 2,7-dihydroxyfluorenone, 3.93g of difluorobenzophenone, 4.14g of anhydrous potassium carbonate, and 90ml of dimethyl sulfoxide and 10ml toluene, nitrogen gas was introduced, stirred for 10min, heated to 160°C, and reacted for 6h. The reaction solution was lowered to room temperature, filtered, the filtrate was added to distilled water, filtered, the precipitate was washed with water and methanol several times, and dried in vacuum to obtain 8.24 g of polyethersulfone ketone with a yield of 72%.
[0016] Add 3.24g of 37% formaldehyde solution into a three-necked flask, add 15ml of dioxane, and stir for 30min. 1.46 g of n-butylamine was dissolved in 15 ml of dioxane. 2.5 g of polyethersulfone ketone was added to the reaction solution, the temperature was raised to 110° C., the reaction was carried out for 6 hours, and the reaction solution was cooled to room temperature. The reaction solution was added to ethanol, the precipitate was filtered, washed several...
Embodiment 2
[0020] Replace n-butylamine with methylamine of the same molar mass, and other conditions are the same as in Example 1.
[0021] H NMR test results (500M, CDCl 3 , ppm): 1.86ppm is the methyl proton peak connected to the oxazine ring, other results are the same as in Example 1. Infrared spectrum test results (KBr, cm -1 ): 3056 is a methyl asymmetric stretching vibration peak, and other results are the same as in Example 1. Curing and testing process are identical with embodiment 1, and the Tg of the obtained polyethersulfone ketone telechelic benzoxazine resin is 253 ℃, T 5 448°C, C 800 was 58.0%.
Embodiment 3
[0023] N-butylamine is replaced by octylamine, and other conditions are the same as in Example 1.
[0024] H NMR test results (500M, CDCl 3 , ppm): δ=0.87~2.42ppm is attributed to the proton peaks of methyl and methylene groups in the octyl structure, and other results are the same as in Example 1. Curing and testing process are identical with embodiment 1, and the Tg of the obtained polyethersulfone ketone telechelic benzoxazine resin is 231 ℃, T 5 410°C, C 800 was 40.0%.
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