Method for preparing graphite oxide
A graphite and hydrogen peroxide technology, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve problems such as high viscosity of the system, graphite expansion, preparation failure, etc., to reduce viscosity, avoid graphite expansion, and reduce severe exothermic conditions Effect
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[0014] Graphite oxide preparation method provided by the invention, such as figure 1 Shown, its process preparation steps are as follows:
[0015] S1. Cool 203-460mL of concentrated sulfuric acid to 0°C with an ice bath;
[0016] S2, join the graphite with purity 99.5% in the concentrated sulfuric acid, then slowly add potassium permanganate (KMnO 4 ), and control the reaction temperature 0 ~ 20 ℃ (preferably 10 ℃), followed by heat preservation and stirring reaction 2 ~ 4h (preferably 3h); wherein, graphite and KMnO 4 The mass ratio is 1:3; among them, graphite and KMnO 4 The mass of each is 20g and 60g;
[0017] S3. The temperature of the reaction system in step S2 is raised to 35±3°C, that is, the temperature is kept and stirred at 32-38°C for 0.5-1 hour;
[0018] S4. Slowly pour the reaction system in step S3 into 460-920mL of water at a temperature of 20-80°C, and control the temperature of the reaction system to be less than 100°C (such as 10°C, 20°C, 40°C, 60°C, 70°...
Embodiment 1
[0024] S1. Cool 460mL of concentrated sulfuric acid to 0°C with an ice bath;
[0025] S2. Add 20g of graphite with a purity of 99.5% to concentrated sulfuric acid, then slowly add 60g of KMnO 4 , and control the reaction temperature at 0°C, then keep stirring and react for 4 hours;
[0026] S3. The temperature of the reaction system in step S2 is raised to 38°C, and the temperature is kept and stirred for 1 hour;
[0027] S4. Slowly pour the reaction system in step S3 into 460 mL of water at a temperature of 20° C., and control the temperature of the reaction system at 20° C., and insulate and stir the reaction for 15 minutes; then, add a concentration of 30 wt % hydrogen peroxide (H 2 o 2 ) until the reaction system does not produce gas; then filter while hot to obtain the solid product, and use a large amount of concentration to wash the solid product with hydrochloric acid of 10wt% to the filtrate without SO 4 2- Finally, wash with water, filter with suction, and dry th...
Embodiment 2
[0029] S1. Cool 230mL of concentrated sulfuric acid to 0°C by means of ice bath cooling;
[0030] S2. Add 20g of graphite with a purity of 99.5% to concentrated sulfuric acid, then slowly add 60g of KMnO 4 , and control the reaction temperature to 20°C, then keep stirring and react for 2h;
[0031] S3. The temperature of the reaction system in step S2 is raised to 35° C. and stirred for 0.5 h;
[0032] S4. Slowly pour the reaction system in step S3 into 700 mL of water at a temperature of 80° C., and control the temperature of the reaction system at 60° C., and keep stirring for 30 minutes; then, add a concentration of 30 wt % hydrogen peroxide (H 2 o 2 ) until the reaction system does not produce gas; then filter while hot to obtain the solid product, and use a large amount of concentration to wash the solid product with hydrochloric acid of 10wt% to the filtrate without SO 4 2- Finally, wash with water, filter with suction, and dry the solid product in a vacuum oven at 5...
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