Polyimide based on diamine monomer containing naphthalimide group and preparation method of polyimide
A technology of naphthalimide group diamine and polyimide is applied in the field of polyimide and its preparation based on naphthalimide group-containing diamine monomer, which can solve the limitation of material application, polyether The heat resistance of the imide is reduced, and it is difficult to melt or dissolve the processing. It achieves the effect of good solubility and improved heat resistance.
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[0044] The preparation method that contains naphthalimide group diamine monomer is as follows:
[0045]
[0046] The specific preparation method takes the following monomer as an example:
[0047]
[0048] Under nitrogen protection, 4-bromonaphthalene anhydride (2.771g, 10.0mmol), hydrazine hydrate (1.5010g, 30.0mmol), and 50mL of ethanol were heated and stirred at 80°C for 4 hours, cooled to room temperature, filtered to obtain a solid, washed with ethanol, and dried 2.7613 g of the intermediate product N-amino-4-bromonaphthalimide was obtained, and the yield was 95%.
[0049] Under nitrogen protection, N-amino-4-bromonaphthalimide (10.7110g, 36.8mmol), 4-aminothiophenol (9.6396g, 77.0mmol), potassium carbonate (10.6712g, 77.3mmol) in 200mL In a mixture of acetonitrile and N,N-dimethylformamide (4:1), heat and stir at 120°C for 10 hours, precipitate solids from the solution in water, and filter to obtain the product N-amino-4-(4-aminobenzene Thio)naphthalimide 11.1070...
Embodiment 1
[0051] In the present embodiment, the reaction formula of polyimide is as follows:
[0052]
[0053] The specific preparation method is: under the protection of nitrogen, add the diamine monomer (4.0mmol) containing naphthalimide group and 16 milliliters of N-methylpyrrolidone into a 50mL reaction bottle, stir at room temperature, and wait until the diamine monomer is completely dissolved Afterwards, biphenyltetralic acid dianhydride (4.0 mmol) was added, and stirring was continued at room temperature for 24 hours to obtain a viscous polyamic acid solution, which was then diluted to a concentration of 10% by weight. Apply the diluted polyamic acid solution evenly on a clean glass plate, the thickness of the solution coating film is 0.5mm, place the glass plate in a drying oven, and heat up according to the following procedure: 80°C, 1 hour; 150°C, 1 hour; 250°C, 1 hour; 300°C, 1 hour. After the temperature dropped to room temperature, the glass plate was taken out, placed ...
Embodiment 2
[0055] In the present embodiment, the reaction formula of polyimide is as follows:
[0056]
[0057]The specific preparation method is: under the protection of nitrogen, add the diamine monomer (4.0mmol) containing naphthalimide group and 16 milliliters of N-methylpyrrolidone into a 50mL reaction bottle, stir at room temperature, and wait until the diamine monomer is completely dissolved Afterwards, bisphenol A dianhydride monomer (4.0 mmol) was added, and stirring was continued at room temperature for 24 hours to obtain a viscous polyamic acid solution, which was then diluted to a concentration of 10% by weight. Then, a mixed solution of 4 mL of acetic anhydride and 2 mL of pyridine was added, and stirring was continued at room temperature for 24 hours to obtain a polyimide solution. Drop the reaction solution into ethanol to obtain fibrous polyimide precipitates, and dry to obtain polyimide powder. The glass transition temperature of the polymer powder is 302°C.
[0058...
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