Diamine monomer containing adamantane structure, polyimide film, its preparation method and application
A technology of polyimide film and diamine monomer is applied in the field of colorless transparent polyimide film and its preparation, and achieves the effects of high yield, easy availability of raw materials and good heat resistance.
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[0045] Another aspect of the embodiments of the present invention provides a method for preparing a diamine monomer containing an adamantane structure, which includes:
[0046] The first homogeneous mixed reaction system comprising 1-adamantanol, acetanilide and / or acetanilide derivatives and a catalyst is subjected to a Friedel-Crafts alkylation reaction at 20-35°C for 2-10 hours to obtain a bisamide compound;
[0047] And, reacting the second homogeneously mixed reaction system comprising the bisamide compound, inorganic base and solvent at 80-130° C. for 6-24 hours to prepare a diamine monomer containing an adamantane structure.
[0048] In some more specific embodiments, the catalyst includes concentrated sulfuric acid, but is not limited thereto.
[0049] Further, the concentration of the concentrated sulfuric acid is 98wt%.
[0050] Further, the molar ratio of the 1-adamantanol to acetanilide and / or acetanilide derivatives is 1:2˜1:2.3.
[0051] Further, the molar rati...
Embodiment 1
[0110] (1) 1-adamantanol (3.75g) and acetanilide (7.8g) are added in the 100mL three-neck round-bottomed flask equipped with mechanical stirring and condenser, then add 37.5mL concentrated sulfuric acid (98wt%), the mixed system is in Stir and react at 20°C for 10 hours. After the reaction is completed, slowly pour the reaction mixture into 100 mL of deionized water, and stir to form a white precipitate. After vacuum filtration, the crude product is washed with water, and the white crude product is washed with ethanol / water (1 / 3, volume ratio) recrystallization and vacuum drying (100°C / 10h) to obtain the bisamide compound, namely 1,3-bis(4-acetylaminophenyl)adamantane (6.32g, yield 63.2%), melting point: 274-275°C (See the H NMR spectrum figure 1 );
[0111] (2) Add absolute ethanol (30mL) and 1,3-bis(4-acetylaminophenyl)adamantane (3.0g) obtained in step (1) into a 100mL single-necked round-bottomed flask and stir to dissolve, then add 10mL Sodium hydroxide solution (10wt%)...
Embodiment 2
[0117] (1) Add 1-adamantanol (3.75g) and 2,6-dimethylacetanilide (8.8g) into a 100mL three-necked round-bottomed flask equipped with a mechanical stirrer and a condenser, and then add 37.5mL of concentrated sulfuric acid ( 98wt%), the mixed system was stirred and reacted at 35°C for 2h. After the reaction was completed, the reaction mixed system was slowly poured into 100mL deionized water, and a white precipitate was precipitated after stirring. The crude product was washed by vacuum filtration and washed with ethanol / Water (1 / 3, volume ratio) recrystallization, vacuum drying (100 ℃ / 10h) to get bisamide compound namely 1,3-bis(3,5-dimethyl-4-acetylaminophenyl) adamantane (6.4 g, yield 69%), melting point: 215°C (see image 3 );
[0118] (2) Add ethylene glycol (25mL), 1,3-bis(3,5-dimethyl-4-acetamidophenyl)adamantane (2.5g) obtained in step (1) into a 100mL single-mouth round Stir to dissolve in the bottom flask, then add 10mL of sodium hydroxide solution (50wt%), heat t...
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