Method of preparing graphene by using supercritical CO2 assisted liquid phase stripping
A technology of CO2 and auxiliary liquid, which is applied in the production of graphene, bulk chemicals, nano-carbon, etc., can solve the problems of poor quality and low production efficiency of graphene, and achieve good structural integrity, green production process, and preparation The effect of simple process
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Embodiment 1
[0024] (1) Weighing 60 mg of natural graphite powder and 60 mL of NMP to form a reaction solution with a concentration of 1 mg / mL, and ultrasonically mixing in a water bath for 10 minutes;
[0025] (2) Add the solution to figure 1 In the reaction kettle shown, after heating the reaction kettle to 40°C through the control module, turn on the mechanical stirring (1000rpm) and use the booster pump to pump the CO in the carbon dioxide bottle 2 Pump it into the reaction kettle, and the reaction will start after the pressure reaches 12MPa;
[0026] (3) After reacting for 2 hours, take out the reactor and place it in a water bath to cool to below 25°C, open the exhaust valve to let the CO 2 go through figure 1 After washing the bottle shown, pour the solution into the beaker;
[0027] (4) Ultrasonic disperse the taken-out solution for 45 minutes, pour it into a centrifuge tube and centrifuge at 2500rpm for 30 minutes, and then take the supernatant to obtain a graphene solution wit...
Embodiment 2
[0029] (1) Weigh 210mg of expandable graphite powder and 70mL of NMP to form a reaction solution with a concentration of 3mg / mL, and ultrasonically mix in a water bath for 5 minutes;
[0030] (2) Add the solution to figure 1 In the reaction kettle shown, after heating the reaction kettle to 50°C through the control module, turn on the magnetic stirring (1500rpm) and use the booster pump to remove the CO in the carbon dioxide bottle. 2 Pump it into the reaction kettle, and the reaction will start after the pressure reaches 16MPa;
[0031] (3) After reacting for 4 hours, take out the reaction kettle and place it in a water bath to cool to below 25°C, open the exhaust valve to drain the CO 2 go through figure 1 The indicated scrubber bottle is drained, and the solution is poured into a beaker;
[0032] (4) Ultrasonic disperse the taken-out solution for 45 minutes, pour it into a centrifuge tube and centrifuge at 2500 rpm for 30 minutes, and then take the supernatant to obtain ...
Embodiment 3
[0034] (1) Weigh 300mg of expandable graphite powder and 60mL of DMF to form a reaction solution with a concentration of 5mg / mL, and ultrasonically mix in a water bath for 15 minutes;
[0035] (2) Add the solution to a preheated to 80°C figure 1 In the reactor, open mechanical stirring (2000rpm) and utilize figure 1 The booster pump in the reactor feeds CO into the reactor 2 , the reaction starts after the pressure reaches 20MPa;
[0036] (3) After reacting for 6 hours, take out the reactor and place it in a water bath to cool to below 25°C, open the exhaust valve to drain the CO 2 go through figure 1 The washing bottle is discharged, and the solution is poured into the beaker;
[0037] (4) Ultrasonic disperse the taken-out solution for 60 minutes, pour it into a centrifuge tube and centrifuge at 2500 rpm for 30 minutes, and then take the supernatant to obtain a graphene solution with a concentration of 0.46 mg / mL. Graphene sheets with less than ten layers accounted for 8...
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