A method for removing sulfate radical impurities in graphene oxide synthesis system
A synthetic system and graphene technology, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve the problems of unfavorable industrial production, low efficiency of centrifugal washing, and extremely high requirements for centrifuge speed, and achieve a level suitable for industrial production Effect
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Embodiment 1
[0038] The improved Hummers method of embodiment 1 synthesizes graphene oxide
[0039] Weigh 3g flake graphite on weighing paper with an analytical balance and place it in a 2L beaker, weigh 360ml and 40ml concentrated sulfuric acid and phosphoric acid respectively with a graduated cylinder and add them to the graphite together. Weigh 18g of potassium permanganate in a small beaker and grind it into powder with a mortar, and slowly add it into the mixture while stirring at 0°C. The mixture was then allowed to stir at 50°C for 12 hours. After cooling to room temperature, add 400ml of ice-water mixture, stir rapidly and gradually add 3ml of 30% hydrogen peroxide. After standing for 3 days, a graphene oxide synthesis system was obtained.
Embodiment 2
[0040] Embodiment 2 adopts the sulfate radical washing liquid of calcium hydroxide solution-dichloromethane two-phase system to remove sulfate radical ion
[0041] Take 150ml of dichloromethane and add it to a 500ml beaker, add 32g of calcium hydroxide into water to make a 200ml suspension and pour it on the dichloromethane, you can see that the solution is clearly divided into upper and lower layers, and the upper layer is calcium hydroxide Suspension, the lower layer is dichloromethane. Add 50 ml of the graphene oxide synthesis system obtained in Example 1 to the junction of the two layers through a peristaltic pump without stirring. It was found that a yellow substance had sunk into the bottom layer of dichloromethane, and a white flocculent precipitate was formed in the water layer.
Embodiment 3
[0042] Example 3 XRD detection
[0043] The white flocculent precipitate in the water layer of Example 2 and the yellow substance in the bottom layer of dichloromethane were taken respectively, dried and subjected to XRD test. The results are as follows figure 1 and figure 2 shown.
[0044] from figure 1 It can be seen that the white flocculent precipitate is calcium sulfate, which proves that the sulfate radical impurity in the graphene oxide synthesis system can be removed by the method provided by the invention.
[0045] from figure 2 It can be observed that graphene oxide has a strong diffraction peak at 2θ=12.839, and the interlayer spacing is It can be seen that the interlayer spacing of oxidized graphite obviously increases, because there are a large number of water molecules and oxygen-containing functional groups such as hydroxyl, carboxyl, and epoxy groups between the oxidized graphite layers. There is a diffraction peak at 2θ=43.198, which is a graphene pla...
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