Method for preparing polyimide aerogel through direct vacuum drying
A polyamic acid wet gel and vacuum drying technology, applied in the field of high-performance porous material preparation, can solve the problems of low efficiency and high cost, and achieve the effects of good replacement effect, low solvent amount and excellent thermal stability.
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[0025] Example 1:
[0026] The pyromellitic anhydride was dried in an oven at 200°C for 2 hours to remove moisture. Dissolve 7.089 g of 4,4'-diaminodiphenylmethane in a low-boiling mixed solvent composed of 68 g of tetrahydrofuran and 17 g of methanol, then add 7.8575 g of dried pyromellitic anhydride monomer, and stir at room temperature for 4 hours. Pour into a mold and let it stand for 1 day to obtain a polyamic acid wet gel. Then use acetone as the replacement solvent, and replace acetone every 12 hours. After replacement for 1 day, use tert-butanol as the replacement solvent to replace acetone. The same is replaced every 12 hours. After replacement for 2 days, vacuum dry at room temperature to obtain polyamic acid gas. gel. Then, the polyamic acid aerogel is imidized at a high temperature by a temperature program process of 100°C for 2 hours, 150°C for 2 hours, and 250°C for 2 hours to obtain a block polyimide aerogel. The density of the obtained polyimide aerogel is 0.10...
Example Embodiment
[0027] Example 2:
[0028] The pyromellitic anhydride was dried in an oven at 200°C for 2 hours to remove moisture. Dissolve 7.089 g of 4,4'-diaminodiphenylmethane in a low-boiling mixed solvent composed of 68 g of tetrahydrofuran and 17 g of methanol, then add 7.8575 g of dried pyromellitic anhydride monomer, and stir at room temperature for 4 hours. Pour into a mold and let it stand for 2 days to obtain a wet gel of polyamic acid, and then use acetone as the replacement solvent to replace the acetone every 12 hours. After replacement for 1 day, use tert-butanol as the replacement solvent to replace acetone, the same every 12 hours Replace it once, after 2 days of replacement, vacuum dry at room temperature to obtain polyamic acid aerogel, and then perform high-temperature imineization on polyamic acid aerogel by temperature-programming process at 100°C for 2 hours, 150°C for 2 hours, and 250°C for 2 hours. To obtain block polyimide aerogel. The density of the obtained polyimi...
Example Embodiment
[0029] Example 3:
[0030] The pyromellitic anhydride was dried in an oven at 200°C for 2 hours to remove moisture. Dissolve 7.089 g of 4,4'-diaminodiphenylmethane in a low-boiling mixed solvent composed of 68 g of tetrahydrofuran and 17 g of methanol, then add 7.8575 g of dried pyromellitic anhydride monomer, and stir at room temperature for 4 hours. Pour into the mold and let it stand for 3 days to obtain a wet gel of polyamic acid, and then use acetone as the replacement solvent to replace the acetone every 12 hours. After replacement for 1 day, use tert-butanol as the replacement solvent to replace acetone, the same every 12 hours Replace it once, after 2 days of replacement, vacuum dry at room temperature to obtain polyamic acid aerogel, and then perform high-temperature imineization on polyamic acid aerogel by temperature-programming process at 100°C for 2 hours, 150°C for 2 hours, and 250°C for 2 hours. To obtain block polyimide aerogel. The density of the obtained polyi...
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