A kind of preparation method of graphene microsphere
A technology of graphene and microspheres, which is applied in the field of preparing graphene microspheres by inverse emulsion method, which can solve the problems that graphene cannot reach a uniform thickness, the size of graphene is limited, and the mechanical strength of graphene balls is low, achieving good application prospects , expanded application, and short process
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Embodiment 1
[0046] The preparation of embodiment 1 graphene oxide
[0047] Add 23mL of concentrated sulfuric acid with a concentration of 98wt% into a dry beaker, cool it to about 0°C in an ice bath, add a solid mixture of 1g graphite powder and 0.5g sodium nitrate, stir, and slowly add 3g potassium permanganate. Stirring and reacting at a temperature of 20°C for 2 hours, the first mixed solution was obtained, and the solution was viscous and dark green;
[0048] Raise the temperature of the first mixed solution to about 35°C, and continue to stir and react for 30 minutes to obtain the second mixed solution, which turns from dark green to brown;
[0049] Continuously and slowly add 46 mL of deionized water dropwise to the second mixed solution, control the temperature at about 100 ° C, continue stirring for 20 min, stop stirring, and then add 3 mL of 30 wt % H 2 o 2 Reducing the residual oxidizing agent to obtain a suspension, the solution turns bright yellow;
[0050] The suspension w...
Embodiment 2
[0052] Use the GO in Example 1 to configure 50 mL of 12 mg / mL GO concentrated solution, and after ultrasonic treatment for 30 min, slowly add ammonia water dropwise until the pH of the solution is 10;
[0053] Prepare a composite oil phase of liquid paraffin and carbon tetrachloride, wherein the volume ratio of liquid paraffin and carbon tetrachloride is 8:1, and the volume of the oil phase is prepared according to 4.5 times the volume of GO;
[0054] A certain amount of (Z)-mono-9-octadecenoic acid sorbitan ester is added to the oil phase, the amount added accounts for 5% of the total volume of the water phase and the oil phase;
[0055] After the oil phase and the water phase are mixed, they are stirred by a homogenizer at 3000 R / min, added to a three-necked bottle, and mechanically stirred for 30 minutes. After the emulsion is stable, hexamethylenediamine is added. The quality of hexamethylenediamine accounts for 35% of the solid content of GO. React for 5 hours at 80°C and...
Embodiment 3
[0060] The GO in Example 1 was used to prepare a 12 mg / mL GO concentrated solution, and after ultrasonic treatment for 30 min, ammonia water was slowly added dropwise until the pH of the solution was 9.
[0061] Prepare a composite oil phase of liquid paraffin and carbon tetrachloride, the volume ratio of liquid paraffin and carbon tetrachloride is 10:1, and the volume of the oil phase is prepared according to 3 times the volume of GO;
[0062] A certain amount of polyoxyethylene sorbitan monooleate is added to the oil phase of the configuration, and the amount added accounts for 3% of the total volume of the water phase and the oil phase;
[0063] After the oil phase and the water phase are mixed, they are stirred by a homogenizer at 3500 R / min, added to a three-necked bottle, and mechanically stirred for 30 minutes. After the emulsion is stable, phenylenediamine is added, wherein the quality of phenylenediamine accounts for 20% of the solid content of GO, and then React at 5...
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