Preparation method of polyimide copolymer having backbone containing anthraquinone structure and composite material thereof
A technology of polyimide copolymer and polyimide products, which is applied in the field of preparation of corresponding carbon nano-composite materials, can solve the problems of difficult disposal of waste liquid, large pollution, high synthesis cost, etc., to increase molecular chains, improve mechanical Performance, Convenience and Affordability
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Embodiment 1
[0025] Take a 100ml dry three-neck flask and fix it on the support of the booster electric mixer, adjust it to be stable, and then pass in N2, remove the air in the bottle, and add the weighed purified and dried diamine monomer 4,4′-diamine after about 5 minutes Aminodiphenyl ether (4,4'-ODA) 1.669g (8.3mmol) and 2,6-diaminoanthraquinone (2,6-DAAQ) 0.3971g (1.7mmol) powder and 32ml N,N-dimethyl Acetamide (DMAc) was stirred at a certain speed until fully dissolved. Then, 2.1812 g (10 mmol) of pyromellitic anhydride (PMDA) was added to the above solution in 3 batches, and reacted for 4 hours under ice-bath conditions. The reaction obtained solid content is 15%, inherent viscosity η inh = 1.89 polyamic acid solution was vacuum defoamed and evenly scraped with a scraper on a clean and dry flat glass. Afterwards, place the glass plate in an electric blast drying oven at 60°C for 12 hours, and then move it into a muffle furnace at room temperature to 100°C, 100 to 200°C and 200 to...
Embodiment 2
[0027] Accurately weigh 22mg of MWCNTs that has been washed by high-speed centrifugation and fully dried, and add it to a sample bottle containing 15ml of DMAc solvent. Sonicate in a water bath for 30min, add 0.477g (2mmol) 2,6-DAAQ powder, and continue to sonicate for 30min. use. The DMAc dispersion containing carbon nanotubes with different mass fractions was ultrasonically transferred into a fully dry 100ml three-neck flask for 30 minutes, and nitrogen protection was introduced. After the airflow was stabilized, an appropriate amount of diamine ODA powder was added, and mechanically stirred rapidly under ice-bath conditions. Add all the dianhydride PMDA in 3 batches within 2 hours, and add all the remaining solvent at the end of the addition to wash away a small amount of reactant sticking to the bottle wall. After vacuum degassing, the polyamic acid solution obtained by the reaction is evenly scraped and coated on a clean and dry flat glass with a scraper. Afterwards, pla...
Embodiment 3
[0029] Take an appropriate amount of polyamic acid in Example 1, make it into a solution with a solid content of 8%, and prepare a nanofiber membrane through a high-voltage electrospinning device under the conditions of 25kV and 50°C. Then place it in an electric blast drying oven at 60°C for pre-baking for 12 hours, and then move it into a muffle furnace at a rate of 3°C / min at room temperature to 100°C, 100 to 200°C and 200 to 300°C. Raise the temperature, keep it warm at the end temperature of each stage for 30 minutes, and take it out after naturally cooling to room temperature with the furnace to obtain a polyimide nanofiber membrane.
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