Graphene aerogel and preparation method and application thereof
A graphene aerogel, graphene hydrogel technology, applied in graphene, electrical components, magnetic field/electric field shielding and other directions, can solve the problems of poor crystallization, fine embedded particle size, and difficulty in deep processing and application of microcrystalline graphite, Achieve the effect of reducing process steps, realizing industrial production and saving preparation time
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reference example 1
[0075] Preparation of graphene oxide:
[0076] 1) Low-temperature pre-oxidation: Add 1.5g of microcrystalline graphite powder and 1.5g of sodium nitrate powder into 40mL of concentrated sulfuric acid, and stir and react in an ice-water bath at 0°C for 1 hour to obtain a low-temperature pre-oxidized graphite solution;
[0077] 2) Low-temperature oxidation: Divide 4.5g of potassium permanganate into 4 parts, and add it to the low-temperature pre-oxidized graphite solution obtained in step 1) every 30 minutes, and stir and react in an ice-water bath at 0°C for 2 hours to obtain a low-temperature oxidized graphite solution;
[0078] 3) Medium-temperature oxidation: Put the low-temperature oxidized graphite solution obtained in step 2) into a three-necked flask, stir and react in a medium-temperature water bath at 38°C for 20 hours, and then add 150 mL of deionized water dropwise under constant temperature conditions. The dropping speed of water is 0.3mL / s, when the volume of addi...
Embodiment 1
[0084] (1) Pre-reduction treatment: Add 30 mg of L-ascorbic acid to 10 mL of the graphene oxide solution (pH=5.5) obtained in Reference Example 1 with a mass concentration of 3 mg / mL and mix. The pH value after mixing is 5.6. No adjustment is required. 150W, frequency 40kHz, after ultrasonic dispersion for 5 minutes, pre-reduction treatment was carried out at 80°C for 30 minutes to obtain a semi-reduced graphene hydrogel;
[0085] (2) Final reduction treatment: Add 90 mg of L-ascorbic acid to the semi-reduced graphene hydrogel obtained in step (1), and perform ultrasonic treatment for 1 min at a power of 150 W and a frequency of 40 kHz, and then proceed at 80 ° C. Final reduction treatment for 30 minutes to obtain graphene hydrogel;
[0086] (3) Alkali soaking: Soak the graphene hydrogel obtained in step (2) in a 0.12mol / L potassium hydroxide solution for 3 hours, and replace it with a fresh 0.12mol / L potassium hydroxide solution every 1 hour to continue Soak and wash the hyd...
Embodiment 2
[0094] (1) Pre-reduction treatment: Add 60 mg of L-ascorbic acid to 10 mL of the graphene oxide solution (pH=5.5) obtained in Reference Example 1 with a mass concentration of 3 mg / mL and mix. The pH value after mixing is 5.7. No adjustment is required. 180W, frequency 40kHz, after ultrasonic dispersion for 5 minutes, pre-reduction treatment was carried out at 80°C for 60 minutes to obtain a semi-reduced graphene hydrogel;
[0095] (2) Final reduction treatment: Add 60 mg of L-ascorbic acid to the semi-reduced graphene hydrogel obtained in step (1), and perform ultrasonic treatment for 1 min at a power of 180 W and a frequency of 40 kHz, and then proceed at 80 ° C. Final reduction treatment for 60 minutes to obtain graphene hydrogel;
[0096] (3) Alkali soaking: Soak the graphene hydrogel obtained in step (2) in a 0.1mol / L sodium hydroxide solution for 4 hours, and replace it with a fresh 0.1mol / L sodium hydroxide solution every 1 hour to continue Soak and wash the hydrogel un...
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