Polyimide-based composite aerogel, controllable preparation method thereof and application of aerogel
A composite aerogel, polyimide-based technology, applied in the field of polyimide-based composite aerogel materials and their controllable preparation, can solve the problems of poor thermal stability, flammability, poor mechanical properties, etc. Improve the effect of mechanics, low cost and ingenious design ideas
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Example Embodiment
[0030] Example 1
[0031] This embodiment includes the following steps:
[0032] Take 30 mL of deionized water, add 2 g of polyamic acid and 1 g of triethylamine, sonicate for 1 h, and stir for 0.5 h to dissolve and disperse the polyamic acid uniformly to obtain an aqueous polyamic acid solution. The polyamic acid hydrogel is obtained through the sol-gel process.
[0033] The obtained polyamic acid hydrogel was transferred to a mold and sonicated for 0.5h, then the mold was transferred to a refrigerator at about 4°C for pre-cooling for 5h, and then put into liquid nitrogen to quickly freeze into a solid, and then Freeze drying for 48 hours under a vacuum of 10-20 Pa to obtain a polyamic acid aerogel.
[0034] Place the obtained polyamic acid aerogel in a tube furnace, and control the heating program in a nitrogen atmosphere, that is, from room temperature to 100°C, heating for 30 minutes and holding for 1 hour; 100°C to 200°C, heating for 30 minutes, holding for 1 hour; 200°C When t...
Example Embodiment
[0035] Example 2
[0036] This embodiment includes the following steps:
[0037] Take 2g of untreated carbon nanotubes, add 300mL of concentrated sulfuric acid and 100mL of concentrated nitric acid, and stir at 70°C for 2h. It was repeatedly washed with 8% hydrochloric acid solution and deionized water, and then freeze-dried to obtain acidified carbon nanotubes, denoted as a-CNT.
[0038] Take 30 mL of 2 mg / mL a-CNT dispersion, add 2 g of polyamic acid and 1 g of triethylamine, ultrasonicate for 1 h, and stir for 0.5 h to dissolve and disperse the polyamic acid uniformly to obtain an acidified carbon nanotube polyamic acid aqueous solution. Then, an acidified carbon nanotube polyamic acid hydrogel is obtained through a sol-gel process.
[0039] The remaining steps are the same as in Example 1. The acidified carbon nanotube polyimide-based composite aerogel was obtained, which was recorded as PI / a-CNT. Through X-ray electron spectroscopy (XPS) and thermal weight loss analysis (TGA) ...
Example Embodiment
[0040] Example 3
[0041] This embodiment includes the following steps:
[0042] Take 2g of untreated carbon nanotubes, add 300mL of concentrated sulfuric acid and 100mL of concentrated nitric acid, and stir at 70°C for 2h. It was repeatedly washed with 8% hydrochloric acid solution and deionized water, and then freeze-dried to obtain acidified carbon nanotubes, denoted as a-CNT.
[0043] Take 30 mL of 2 mg / mL a-CNT dispersion, add 11 μL of 50 wt% hydrazine hydrate and 75 μL of 25 wt% ammonia, and stir at 95° C. for 0.5 h. An acidified-aminated carbon nanotube dispersion liquid is obtained.
[0044] Take 30mL of 2mg / mL acidified-aminated carbon nanotube dispersion, add 2g of polyamic acid and 1g of triethylamine, sonicate for 1h, and stir for 0.5h to dissolve and disperse the polyamic acid uniformly to obtain acidified-aminated carbon nanotubes Tube polyamic acid aqueous solution. Then, an acidified-aminated carbon nanotube polyamic acid hydrogel is obtained through a sol-gel proce...
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