Dianhydride monomer containing 2,5-furandimethanol residues, and preparation method thereof, and polyimide film and preparation method thereof
A technology of polyimide film and furan dimethyl residue is applied in the field of polyimide film and its preparation, which can solve the problems of poor biodegradability, not conforming to green sustainable development and the like, and achieves good solubility, The effect of improving processing conditions and recycling rate
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[0042] The present invention also provides the preparation method of the dianhydride monomer containing 2,5-furandimethanol residue described in the above technical scheme, comprising the following steps:
[0043] Mixing 2,5-furan dimethyl derivative, dicyano compound, first base and solvent to undergo substitution reaction to obtain tetracyano compound;
[0044] Mixing the tetracyano compound, the second base, the phase transfer catalyst and water for a hydrolysis reaction to obtain a tetraacid containing a 2,5-furandimethanol structure;
[0045] Mixing the tetraacid containing 2,5-furandimethanol structure and acetic anhydride for a decarboxylation reaction to obtain the dianhydride monomer containing 2,5-furandimethanol residue;
[0046] The 2,5-furan dimethyl derivative is
[0047] In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.
[0048] In the present invent...
Embodiment 1
[0093]Under the conditions of normal temperature and pressure and stirring, 100mmol 2,5-furandimethanol, 205mmol 4-nitrophthalonitrile, 205mmol sodium hydride and 1mol N,N-dimethylformamide were mixed, and the Biotage Initiator+microwave The reaction occurred in the synthesizer (80°C, 10min). During the reaction, the completion of the reaction was detected by thin-layer chromatography on silica gel GF254. After cooling down to room temperature, it was poured into deionized water, and the alkaline solution was recovered and the precipitated solid was extracted. Filtered, washed 3 times with deionized water, dried in vacuum (80°C, 12h), and recrystallized with acetonitrile to obtain
[0094] 50mmol Mix 600mmol potassium carbonate, 500mmol 18-crown-6 and 1mol water, raise the temperature to reflux, and filter while hot to remove insoluble impurities after 1h, pour the filtrate into deionized water to precipitate precipitate after cooling, suction filter, vacuum dry (80°C ,12h...
Embodiment 2
[0099] Under the conditions of normal temperature and pressure and stirring, 100mmol 220mmol 4-nitrophthalonitrile, 220mmol potassium hydride and 600mmol dimethyl sulfoxide were mixed and reacted in a microwave reactor modified from a domestic microwave oven (100°C, 30min). Silica gel GF254 was used to detect the completion of the reaction, lowered to room temperature, poured into deionized water, recovered the alkaline solution and filtered the precipitated solid with suction, washed 5 times with deionized water, dried in vacuum (80°C, 12h), washed with acetonitrile recrystallized to obtain
[0100] 50mmol Mix 800mmol potassium carbonate, 750mmol 15-crown ether-5 and 1.1mol water, heat up to reflux, filter while hot to remove insoluble impurities after 1h, pour the filtrate into deionized water to precipitate precipitate after cooling, suction filter, vacuum dry (80 ℃, 12h), recrystallized with acetonitrile to obtain
[0101] 20mmol and 1.6mol acetic anhydride, hea...
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