Process for producing polybenzoxazole film
A technology of polybenzoxazole film and polybenzoxazole, applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve insufficient dispersion, insufficient dispersion of carbon nanotubes, The characteristics have not been improved and other problems, to achieve the effect of high solubility
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Embodiment 1
[0119] Manufacture of tert-butoxycarbonyl-substituted polyamides (1)
[0120] (i) Under a dry nitrogen atmosphere, add 4.29g of N,N',O,O'-tetrakis(trimethylsilyl)-4,6-diaminoresorcinol produced in the reference example to a 300ml three-necked flask (10 mmol) and 20 ml of dehydrated N-methyl-2-pyrrolidone were dissolved at 0°C. 2.03 g (10 mmol) of purified commercially available terephthaloyl chloride was added in small amounts and reacted at 0° C. for 6 hours. After the reaction was completed, the reaction solution was added dropwise to 1000 ml of methanol, and the precipitate was collected by filtration and washed with 100 ml of methanol. Intrinsic viscosity η of sediment inc It is 1.21dl / g. By infrared absorption spectroscopy ( image 3 ) to identify the structure and confirm the formation of polyamide.
[0121] (ii) 0.48 g (2 mmol) of the polyamide synthesized in (i), 5 ml of N-methyl-2-pyrrolidone, and 3 ml (8 mmol) of triethylamine were added to a 50 ml two-necked fl...
Embodiment 2
[0123] Manufacture of tert-butoxycarbonyl-substituted polyamides (2)
[0124] (i) Under a dry nitrogen atmosphere, add 4.29g of N,N',O,O'-tetrakis(trimethylsilyl)-4,6-diaminoresorcinol produced in the reference example to a 300ml three-necked flask (10 mmol) and 20 ml of dehydrated N-methyl-2-pyrrolidone were dissolved at 0°C. 2.03 g (10 mmol) of purified commercially available terephthaloyl chloride was added in small amounts and reacted at 0° C. for 6 hours.
[0125] (ii) Next, 50 ml of N-methyl-2-pyrrolidone was added to the reaction liquid, followed by further stirring for 1 hour. 8.3 ml (60 mmol) of triethylamine and 9.2 ml (40 mmol) of di-tert-butyl dicarbonate were added to the reaction solution, and the reaction was continued for 24 hours. After the reaction, the reaction solution was added dropwise into 1000 ml of methanol, and the precipitate was collected by filtration and washed with 100 ml of methanol to obtain a tert-butoxycarbonyl-substituted polyamide. Yield...
Embodiment 3
[0127] Fabrication of polybenzoxazole membranes
[0128] (i) 0.5 g of tert-butoxycarbonyl-substituted polyamide produced in Example 2 was dissolved in 100 ml of N-methyl-2-pyrrolidone to prepare a casting solution, and the solution was cast on an aluminum plate of 5 cm×5 cm. Thereafter, the solvent was distilled off under an environment of 3 mmHg at room temperature for 24 hours, and then at 3 mmHg for 1 hour at 100° C., 200° C., and 300° C., respectively, to obtain a polyamide film.
[0129] (ii) Next, the polyamide film was heated together with the plate at 360° C. for 30 minutes under a nitrogen stream to convert the polyamide to polybenzoxazole, thereby obtaining a polybenzoxazole film. The infrared absorption spectrum of the obtained film is shown in Figure 6 . Also, the TGA chart when the casting solution used in (i) was heated to 700°C is shown in Figure 7 . As a result of examining the mechanical properties of the obtained polybenzoxazole film, it was found that ...
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