A method for preparing graphene by exfoliating three times with ultrasonic wave, supercritical CO2 and microwave
A supercritical and ultrasonic technology, applied in graphene, chemical instruments and methods, and bulk chemical production, etc., can solve the problems of low quality graphene, reduced graphene performance, and inability to industrialize large-scale mass production. Inexpensive, low number of layers, high carbon content
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Embodiment 1
[0050] Weigh 10 g of graphite flakes, add 300 ml of 98% concentrated sulfuric acid and stir at 0-5° C. for 30 min. Add 0.8g potassium permanganate and raise the temperature to 60°C for 6h. The reaction solution was filtered with suction, and the solid was filtered out and washed with water until neutral. Dry at 80°C for 2h.
[0051] Add the dried intercalated graphite into a 200ml ball mill jar, grind for 1 hour and sieve, and grind to a particle size of 150 mesh.
[0052] The dried expanded graphite was dispersed in 300ml of N-methylpyrrolidone, and the temperature of the solution was set to 30°C in an ultrasonic cleaning machine, and the ultrasonic power was 400W for 10 hours.
[0053] The solution after ultrasonic treatment was suction filtered, and the filtered solid was put into supercritical CO 2 The pressure in the reactor was adjusted to 20MPa, the temperature was raised to 200°C, and the supercritical treatment was performed for 2 hours.
[0054] The treated pre-e...
Embodiment 2
[0056] Weigh 10 g of artificial graphite, add 300 ml of 98% concentrated sulfuric acid and stir at 0-5°C for 30 min. Add 0.8g potassium permanganate and raise the temperature to 60°C for 6h. The reaction solution was filtered with suction, and the solid was filtered out and washed with water until neutral. Dry at 80°C for 2h.
[0057] Add the dried intercalated graphite into a 200ml ball mill jar, grind for 1 hour and sieve, and grind to a particle size of 150 mesh.
[0058] The dried expanded graphite was dispersed in 300ml of N-methylpyrrolidone, and the temperature of the solution was set to 30°C in an ultrasonic cleaning machine, and the ultrasonic power was 500W for 4 hours.
[0059] The solution after ultrasonic treatment was suction filtered, and the filtered solid was put into supercritical CO 2 The pressure in the reactor was adjusted to 15MPa, the temperature was raised to 150°C, and the supercritical treatment was performed for 2 hours.
[0060] The treated pre-...
Embodiment 3
[0062] Weigh 10 g of graphite flakes, add 300 ml of a mixed solution of 98% concentrated sulfuric acid and concentrated nitric acid, the ratio is 5-8:1, control the temperature at 0-5°C and stir for 30 min. Add 0.8g potassium permanganate and raise the temperature to 60°C for 6h. The reaction solution was filtered with suction, and the solid was filtered out and washed with water until neutral. Dry at 80°C for 2h.
[0063] Add the dried intercalated graphite into a 200ml ball mill jar, grind for 1 hour and sieve, and grind to a particle size of 50 mesh.
[0064] The dried expanded graphite was dispersed in 300ml of N-methylpyrrolidone, and the temperature of the solution was set to 30°C in an ultrasonic cleaner, and the ultrasonic power was 500w for 4 hours.
[0065] The solution after ultrasonic treatment was suction filtered, and the filtered solid was put into supercritical CO 2 The pressure in the reactor was adjusted to 20MPa, the temperature was raised to 200°C, and t...
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