Polyfluorene naphthalene aromatic amide, preparation method and applications thereof
A polyfluorene naphthalene aromatic amide and a polymerization reaction technology are applied in the field of polyfluorene naphthalene aromatic amide and its preparation, and can solve the problems of high cost, limited application field of polyaromatic amide materials, large environmental pollution and the like
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[0033] The present invention also provides the preparation method of polyfluorene naphthalene aromatic amide according to the above technical scheme, which includes the following steps:
[0034] Mixing naphthalene dicarboxylic acid, 9,9-bis(4-aminophenyl) fluorene, triphenyl phosphite, organic solvent and co-solvent, polymerization reaction occurs to obtain the polyfluorene naphthalene aromatic amide;
[0035] The naphthalenedicarboxylic acid is 1,4-naphthalenedicarboxylic acid or 2,6-naphthalenedicarboxylic acid.
[0036] In the present invention, the reaction mechanism of the polymerization reaction is:
[0037]
[0038] In the present invention, the molar ratio of the naphthalenedicarboxylic acid, 9,9-bis(4-aminophenyl)fluorene and triphenyl phosphite (TPPi) is preferably 1:1:(3 to 5), more preferably It is 1:1:3. The organic solvent preferably includes N-methylpyrrolidone (NMP) and pyridine; the co-solvent is preferably lithium chloride; the volume ratio of the N-methylpyrrolidon...
Example Embodiment
[0046] Example 1
[0047] Under stirring (150rad / s) conditions, mix 2.2916g (0.0106mol) 1,4-naphthalenedicarboxylic acid, 3.6935g (0.0106mol) 9,9-bis(4-aminophenyl) fluorene, 4.74g (4ml ) After mixing LiCl and 6mLTPPi (0.0318mol), add 30mLNMP and 10mL pyridine, heat up to 90°C, react for 2 hours, wait until the system becomes a slightly viscous light yellow solution; warm up to 110°C, the system gradually changes from viscous to thinner. It becomes viscous again while speeding up the stirring speed (350rad / s). After continuing the reaction for 8 hours, stop stirring and heating, and slowly pour the resulting product system into methanol at room temperature to allow cooling and precipitation to obtain a thin strip-like solid; The thin solids are filtered and crushed; the crushed powder is boiled and washed with methanol for 10 times, and then washed with deionized water for 5 times, and the washed powder is dried in an oven for 12 hours to obtain the polyfluorene naphthalene aroma...
Example Embodiment
[0048] Example 2
[0049] Under stirring (150rad / s) conditions, 1.7079g (0.0079mol) 1,4-naphthalene dicarboxylic acid, 2.7527g (0.0079mol) 9,9-bis(4-aminophenyl) fluorene, 4.74g (4ml ) After mixing LiCl and 8mLTPPi (0.0237mol), add 30mLNMP and 10mL pyridine, heat up to 90℃, react for 2 hours, wait until the system becomes a slightly viscous light yellow solution; when heated to 110℃, the system gradually changes from viscous to thinner. It becomes viscous again while speeding up the stirring speed (350rad / s). After continuing the reaction for 6 hours, stop stirring and heating, and slowly pour the resulting product system into methanol at room temperature to allow cooling and precipitation to obtain a thin strip of solid; The fine strip solids are filtered and pulverized; the pulverized powder is boiled and washed with methanol for 6 times, and then washed with deionized water for 6 times, and the washed powder is dried in an oven for 12 hours to obtain the polyfluorene naphthale...
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