Normal-pressure preparation method of high specific surface area intensive-hydrophobicity graphene oxide/silica composite aerogel
A high specific surface area, composite aerogel technology, applied in the direction of chemical instruments and methods, carbon compounds, silicon compounds, etc., can solve the problems of restricting the application of freeze-drying method, affecting the polycondensation process of precursors, and high airgel density. Achieve the effects of improving uneven pore size, shortening gel time, and high specific surface area
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[0052] Example 1
[0053] Ethyl orthosilicate, ethanol, and water were mixed in a molar ratio of 1:7:2, and after stirring at room temperature for 20 minutes, diluted hydrochloric acid was added dropwise to the mixed solution to pH=2, and the mixture was reacted for 8 hours at room temperature. DMF was added dropwise to the mixed solution, where the mass ratio of DMF to ethyl orthosilicate was 0.15:1. After stirring for 30 minutes, the ethanol solution of aminopropyltriethoxysilane was added dropwise to pH=6. Drop 0.018g of graphene oxide hydrosol with a mass fraction of 5%, sonicate for 30 minutes at a temperature of 20°C at a power of 50W, and continue to drop an ethanol solution of aminopropyltriethoxysilane into the mixed solution to pH =7.2, placed in an ultrasonic cleaner for 8 minutes to form a gel.
[0054] The formed alcogel was aged for 12 hours at room temperature, and then aged with a 20% water / ethanol mixture and a 20% ethyl orthosilicate / ethanol mixture for 24 hours,...
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[0056] Example 2
[0057] Ethyl orthosilicate, ethanol, and water were mixed in a molar ratio of 1:14:2, and after stirring at room temperature for 25 minutes, dilute hydrochloric acid was added dropwise to the mixed solution to pH=2.5, and the mixture was reacted for 16 hours at room temperature. After adding DMF dropwise to the mixed solution and stirring for 30 minutes, the mass ratio of DMF to ethyl orthosilicate was 0.2:1, and the ethanol solution of aminopropyltriethoxysilane was added dropwise to pH=6. Drop 0.18g of graphene oxide hydrosol with a mass fraction of 15%, sonicate it at 25°C for 30 minutes at a power of 60W, and continue to drop the ethanol solution of aminopropyltriethoxysilane into the mixed solution to pH= 7.5. After 12 minutes in an ultrasonic cleaner, a gel is formed.
[0058] The formed alcogel was aged for 18 hours at room temperature, and then aged with a 15% water / ethanol mixture and a 15% ethyl orthosilicate / ethanol mixture for 36 hours, respectively,...
Example Embodiment
[0062] Example 3
[0063] Ethyl orthosilicate, ethanol, and water were mixed in a molar ratio of 1:14:3, and after stirring at room temperature for 30 minutes, dilute hydrochloric acid was added dropwise to the mixed solution to pH=3, and reacted at room temperature for 24 hours. After adding DMF dropwise to the mixed solution and stirring for 30 minutes, the mass ratio of DMF to ethyl orthosilicate is 0.25:1, and the ethanol solution of aminopropyltriethoxysilane is added dropwise to pH=6. Add 0.27g of graphene oxide hydrosol with a mass fraction of 20% dropwise, sonicate it at 30°C for 30 minutes under 80W power, and continue to drop the ethanol solution of aminopropyltriethoxysilane into the mixture to pH=8 , Placed in an ultrasonic cleaner for 18 minutes to form a gel.
[0064] The formed alcogel was aged for 24 hours at room temperature, and then aged with a 25% water / ethanol mixture and a 30% ethyl orthosilicate / ethanol mixture for 18 hours, respectively, with a volume fract...
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