Method for preparing two-dimensional nitrogen-doped graphene in microreactor confined in vertical direction
A technology of nitrogen-doped graphene and micro-reactor, which is applied in the fields of graphene, chemical instruments and methods, catalyst activation/preparation, etc., and can solve problems such as inability to template and mix
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Embodiment 1
[0023] [Example 1] Preparation of ABPBI (method 1, solid-phase method): Take an appropriate amount of 3,4-diaminobenzoic acid (DABA) in a mortar, grind it thoroughly and then transfer it to a three-port chamber equipped with electric stirring and inert gas protection. In the flask, pass nitrogen gas for 15 minutes to exhaust the air in the flask. Under nitrogen protection, under stirring, heat in an oil bath at 225°C for 3 hours. After cooling, take it out, grind it finely, and heat it in an electric furnace under the protection of nitrogen, and raise the temperature to 270-275°C and keep it for 3 hours. After cooling to room temperature, the product was taken out and finely ground to obtain ABPBI, and the molecular weight of ABPBI was measured with an Ubbelohde viscometer.
Embodiment 2
[0024] [Example 2] Preparation of ABPBI (method 2, liquid phase method): polyphosphoric acid (PPA) (50 g) was added into a three-necked flask, and stirred at 160° C. for 1 h under nitrogen protection to remove moisture and air. Add 3,4-diaminobenzoic acid (6 g, 39.5 mmol) and raise the temperature to 200 °C and stir the reaction for 5-8 h. During the reaction, about 5 g P 2 o 5 To absorb the water formed during the reaction. With the increase of reaction time, the polymerization system gradually became viscous. The reaction mixture was slowly transferred to deionized water, spinning to form a fibrous black solid, which was taken out and dried, crushed, and washed to remove polyphosphoric acid and unreacted raw materials in the reaction mixture. Get ABPBI products. The molecular weight of ABPBI was determined with an Ubbelohde viscometer.
Embodiment 3
[0025] [Example 3] Acid modification treatment and cationic surfactant modification of montmorillonite.
[0026] Acid modification of montmorillonite: Take 10 g montmorillonite (Na-MMT) into a 1000mL beaker, add 600 mL of 0.1mol / L HCl, stir, soak for 2 days, filter with suction, and use a large amount of deionized Wash with water several times, filter with suction, and dry at 60°C to obtain acid-modified montmorillonite (H-MMT). Its ion exchange capacity was determined to be 0.25 meq / g.
[0027] Cationic Surfactant C 16 Alkyl dimethyl benzyl ammonium bromide modified montmorillonite (MMT C16B ), weighed 5 g H-MMT (0.25 meq / g), dried at 120~220°C for 2 h to remove the adsorbed water and other impurities, slowly added 0.5 g of C 16 Alkyl dimethyl benzyl ammonium bromide cationic surfactant was dissolved in 300 mL of deionized aqueous solution, fully stirred in a 60°C water bath for 4 hours to make it evenly dispersed, left overnight, suction filtered, and washed with deionize...
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