Method for preparing large-scale graphene through supercritical carbon dioxide exfoliation
A carbon dioxide and supercritical technology, applied in the production of graphene, nano-carbon, bulk chemicals, etc., can solve the problems of high pressure, high toxicity of organic solvents, low output, etc., to increase the number of boost and step-down, and widely used Prospects, effects of huge economic benefits
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Embodiment 1
[0023] A certain amount of sodium lauryl sulfate is mixed with graphite powder, and the weight ratio of graphite powder and sodium lauryl sulfate is 1:5, and is added in the autoclave 4. The autoclave temperature was set at 65°C, and the control temperature was 40°C. The carbon dioxide is pumped into the autoclave 4 by the pump 3, and the pressure in the still is controlled at 18MPa. The material stays in the autoclave 4 for 120 minutes. Through testing and characterization, graphene with less than 10 layers in the product accounts for 42%.
Embodiment 2
[0025] A certain amount of sodium dodecylbenzenesulfonate is mixed with graphite powder, and the weight ratio of graphite powder and sodium dodecylbenzenesulfonate is 1:6, and is added in the autoclave 4 . The material in the autoclave 4 is heated, and the temperature is controlled to 45°C. Carbon dioxide is pumped into the autoclave 4 by the pump 3, and the pressure in the still is controlled at 10MPa. The material stays in the autoclave 4 for 60 minutes. After a quick depressurization, the carbon dioxide is pumped in again through the pump 3. Repeat the pressurization and depressurization process three times. Through testing and characterization, graphene with less than 10 layers in the product accounts for 63%.
Embodiment 3
[0027] Ethanol was used as co-solvent. A certain amount of ethanol is mixed with graphite powder and added to the autoclave 4. The material in the autoclave 4 is heated, and the temperature is controlled to 55°C. Carbon dioxide is pumped in the autoclave 4 by the pump 3, and the pressure in the control kettle is at 12MPa. The material stays in the autoclave 4 for 30 minutes. After a quick depressurization, the carbon dioxide is pumped in again through the pump 3. Repeat the pressurization and depressurization process three times. A certain amount of ethanol is added to the pressure relief tank 7, and the valve is opened to quickly relieve the pressure. According to the test and characterization, the graphene with less than 10 layers in the product accounts for 81%.
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