Preparation method of graphene
A technology of graphene and flake graphite, which is applied in the field of chemical manufacturing, can solve the problems of high cost and low yield, and achieve the effects of simple operation, reduced production cost and improved efficiency
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[0021] The preparation method of graphene comprises the following steps:
[0022] a. React flake graphite, concentrated sulfuric acid and potassium permanganate with a mass ratio of 1:5~6:2~3 at 0~5°C for 30 minutes, then heat to 40~90°C for 20~130 minutes to obtain solidification thing;
[0023] b. Add aqueous hydrogen peroxide solution to the above solidified product, stir for 0.5-2 hours, then filter, wash the solid with water until the pH of the washing liquid is 6-7; make the solid into a suspension of 2-5 g / mL, and ultrasonically crush it for 20-20 40 minutes; wherein, the power of the ultrasonic wave is 200W-400W;
[0024] c. Leave the suspension after ultrasonic crushing for 12 to 48 hours, separate and remove water, until the volume of the suspension is 1 / 2 to 1 / 3 of the original volume, and obtain a concentrate;
[0025] d. Reflux the above-mentioned concentrated solution with hydrazine hydrate for 18-24 hours, after cooling, suction filter and dry to prepare graph...
Embodiment 1
[0036] 100g of flake graphite, concentrated sulfuric acid and potassium permanganate are used as raw materials, and the mass ratio is 1:6:2, and the reaction is carried out in an ice-water bath for 30 minutes. Then heat to 60°C to react, and stop heating after reaching the solidification point in 76 minutes to obtain a cured product.
[0037]Then add 50mL of 30% hydrogen peroxide aqueous solution to the above cured product until no yellow substance is produced (yellow substance is that too much potassium permanganate is reduced to manganese dioxide, its color is generally yellow, and can be used as excess permanganese sign of complete reduction of potassium acid). Then wash with deionized water until the pH of the filtrate is 7. Add water to make a suspension of about 5g / mL, place it in an ultrasonic breaker for ultrasonic crushing for 30 minutes, then let it stand for 48 hours, remove the water in the upper layer, and make the volume 1 / 2 of the original volume. Add hydrazin...
Embodiment 2
[0039] Using 100g of flake graphite, concentrated sulfuric acid and potassium permanganate as raw materials, the mass ratio of which is 1:6:3, the reaction is carried out in a beaker under ice-water bath conditions for 30 minutes. Then heat to 60°C to react, and stop heating after reaching the solidification point in 58 minutes to obtain a cured product.
[0040] Then, 60 mL of 30% hydrogen peroxide aqueous solution was added to the solidified product until no yellow substance was produced. Then wash with deionized water until the pH of the filtrate is 7. Add water to make about 5g / mL aqueous solution (suspension), place it in an ultrasonic breaker for ultrasonic crushing for 30 minutes, then let it stand for 48 hours, remove the water in the upper layer, and make the volume 1 / 2 of the original volume. Add hydrazine hydrate according to the volume of graphene suspension: hydrazine hydrate (80%w / v) volume = 5: 1, heat and reflux for 24h, then suction filter and dry to prepare ...
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