Three-dimensional porous graphene composite material, preparation method and application thereof
A three-dimensional porous and composite material technology, applied in chemical instruments and methods, water treatment of special compounds, physical/chemical process catalysts, etc., can solve problems such as high operating costs, large consumption of chemicals, narrow applicable pH range, etc., to achieve easy Separation and recovery, large specific surface area, mild reaction effect
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[0029] Such as figure 1 Shown, the present invention proposes a kind of preparation method of three-dimensional porous graphene composite material, it is characterized in that, this preparation method comprises the steps:
[0030] (a) Add FeSO dropwise to graphene oxide at room temperature and in the absence of oxygen 4 and Al 2 (SO 4 ) 3 The mixed solution of the mixed solution is stirred evenly to obtain a solid-liquid mixture, wherein the concentration of graphene oxide is preferably 1mg / ml~6mg / ml, and the graphene oxide and FeSO in the mixed solution 4 The mass ratio of Al is preferably 0.4:1 to 4:1, and the Al in the mixed solution 2 (SO 4 ) 3 with FeSO 4 The ratio of the amount of substances is preferably 1:64 to 1:2;
[0031] (b) adding KBH to the solid-liquid mixture prepared in step (a) 4 solution in which KBH 4 FeSO in solution mixed with step (a) 4The ratio of the amount of the substance is 6:1 to 13:1, and it is stirred for 1h to 28h in an oxygen-free en...
Embodiment 1
[0062] First prepare graphene oxide, the specific steps are as follows:
[0063] (i) Mix 1.0g of expandable graphite and 106ml of concentrated sulfuric acid into the reaction vessel, and fully stir in the ice wastewater bath for 30min, then add 5g of potassium permanganate to fully react to obtain a solid-liquid mixture, and keep the solid-liquid The temperature of the mixture does not exceed 15°C;
[0064] (ii) withdraw the solid-liquid mixture prepared in step (i) from the ice wastewater bath, and stir at a constant temperature of 35±1°C for 3 days to fully oxidize the graphite to obtain a precursor;
[0065] (Ⅲ) add ultrapure waste water respectively to the precursor prepared in step (ii) to disperse graphite oxide, add 40ml ultrapure waste water for the first time, and stir at 60±1°C for 60min, add 40ml ultrapure waste water for the second time Pure wastewater, and keep it at 90±1°C for 30min, add 40mL of ultra-pure wastewater directly for the third time, and then add 10m...
Embodiment 2
[0076] Utilize the graphene oxide obtained in embodiment 1 to prepare three-dimensional porous graphene composite material, concrete steps are as follows:
[0077] (a) Ultrasonic disperse 0.6g of graphite oxide with a concentration of 1mg / mL in 100mL of ultrapure wastewater for 3h (temperature 25°C, frequency 40kHz, power 300W), and 0.15g FeSO 4 ·7H 2 O and 0.18g Al 2 (SO 4 ) 3 18H 2 O was dissolved in ultrapure wastewater and the volume was adjusted to 50 mL, then FeSO was added dropwise to graphene oxide at a rate of 1 mL / min under a nitrogen atmosphere. 4 and Al 2 (SO 4 ) 3 Mixed solution, stir to obtain a solid-liquid mixture;
[0078] (b) 0.3784g KBH 4 Dissolve in ultrapure waste water and set the volume to 50ml, add KBH to the solid-liquid mixture prepared in step (a) at a rate of 1mL / min 4 solution, and stirred for a period of time under a nitrogen atmosphere to fully react, and then the resulting precipitate was pre-frozen at -60°C, and then vacuum freeze-dri...
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