Preparation method of graphene oxide
A technology of graphene and graphite, which is applied in the direction of chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of huge usage, achieve wide application prospects, reduce costs, and reduce particle size
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Embodiment 1
[0061] 5g of microcrystalline graphite powder was pretreated by ball milling; after treatment, add 60ml of concentrated sulfuric acid, mix and stir in an ice-water bath for 10min, then add 2g of dry ice, and slowly add 30g of potassium permanganate in batches (about 10min in total), add Observe the temperature of the mixture during the process. When the temperature is higher than 5°C, add dry ice (a total of about 3g of dry ice is added) to keep the solution at around 5°C. Stir at low temperature for 1 hour in an ice-water bath at a speed of 150rpm. Add 1 g of ferric chloride into the solution, continue to stir in an ice-water bath for 1 h, then transfer the solution to a medium-warm water bath at 45° C. and stir for 2 h at a speed of 150 rpm. Take 100ml of ice water and slowly add it into the solution along the wall of the cup, and test the temperature of the solution so that it is not higher than 90°C, the reaction time is 5h, the rotation speed is 150rpm, after natural cooli...
Embodiment 2
[0063] The operation is the same as in Example 1, the difference is that the amount of dry ice to be added later is reduced to 2g, and in order to maintain the condition below 5°C, continue to slow down the addition of KMnO 4 The speed (about 15min) makes the temperature rise slower, and the resulting graphene oxide is designated as sample 2#.
Embodiment 3
[0071] The particle size test was carried out on the samples prepared in the above examples and comparative examples. Figure 1-Figure 5 They are the particle size distribution diagrams obtained by the Malvern laser particle size analyzer. Table 1 is the specific test results. Z-average particle size refers to the average particle size, and PDI refers to the polydispersity index. It can be seen that the Z-average particle diameters of samples 1# and 2# are around 180nm, far smaller than the Z-average particle diameters of samples D1#, D2# and D3#, indicating that the addition of dry ice and ferric chloride can greatly reduce the The particle size of graphene oxide, the PDI of samples 1# and 2# is about 0.27, which is also smaller than the PDI of samples D1#, D2# and D3#.
[0072] The particle size data table of the sample prepared by the embodiment of table 1 and the comparative example
[0073] 1# 2# D1# D2# D3# Z average particle size 174.2nm 183.3...
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