Method for preparing graphene through large-scale aqueous phase
A water-phase preparation, graphene technology, applied in the direction of graphene, nano-carbon, etc., can solve the problems of low packing density of graphene powder, limited dispersion ability, and high energy consumption
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[0046] The preparation process of the present invention includes the following steps:
[0047] (1) Using flake graphite powder, natural graphite powder, synthetic graphite powder or expanded graphite powder as starting materials, intercalation is carried out by oxidation intercalation method to prepare intercalated graphite;
[0048] The oxidant of the oxidation intercalation method described in step (1) can be sulfuric acid, nitric acid, perchloric acid, phosphoric acid, hydrogen peroxide, potassium permanganate, potassium dichromate, chromium trioxide, ammonium persulfate, formic acid, acetic acid, oxalic acid , Bromine, chlorine, iodine chloride, iodine bromide, ozone, oxygen, or any combination between them. , But not limited to this.
[0049] The preparation process of intercalated graphite described in step (1) refers to completion at low temperature, and the purpose is to avoid excessive oxidation of the graphene sheet during the intercalation process. The preferred interca...
Embodiment 1
[0064] Mix 200 ml of concentrated sulfuric acid (98%) with 10 g of potassium permanganate (purity> 95%), 10 grams of flake graphite powder (particle diameter is 500 microns or 35 mesh, carbon content> 95%) uniform mixing, control system temperature below 35 o C. After stirring continuously for 1 hour, slowly add it to 500 ml of ice water, taking care to remove the heat of mixing in time to avoid excessively high system temperature. Then add 20 ml of hydrogen peroxide and stir for 5 minutes, and obtain sulfuric acid intercalated graphite intercalation compound after filtration.
[0065] The sulfuric acid-graphite intercalation compound (wet) obtained after filtration was mixed with 10 g of sodium hydroxide and 250 ml of water. An ultrasonic probe (power 500 W, 95%) was used to obtain a black graphene suspension after 10 minutes. After centrifuging the resulting black solution for 10 minutes at 10,000 revolutions / min, the supernatant was poured to obtain an aqueous paste with high ...
Embodiment 2
[0068] Mix 100 milliliters of fuming sulfuric acid (containing 20% sulfur trioxide), 5 milliliters of hydrogen peroxide, and 10 grams of flake graphite powder (particle diameter of 500 microns) evenly, and pay attention to control the temperature of the system below 35 o C. After stirring continuously for 1 hour, filter, then add to oxalic acid solution and soak for 1 hour, and filter again to obtain intercalated graphite intercalation compound.
[0069] The sulfuric acid-graphite intercalation compound (wet) obtained after filtration was mixed with 10 g of sodium hydroxide and 250 ml of water. A black graphene suspension was obtained after 10 minutes with an ultrasonic probe (power 500W, 95%). After centrifuging the resulting black solution for 10 minutes at 10,000 rpm, the supernatant was poured to obtain an aqueous paste with high graphene content. Compared with graphite raw materials, the yield of graphene is greater than 90%.
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