Preparation method of MOF-derived puffed rice cake-shaped nitrogen-doped porous carbon material
A nitrogen-doped porous carbon and rice cake technology, applied in the preparation/purification of carbon, etc., can solve the problems of staying in the academic research stage and limiting practical applications.
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Embodiment 1
[0024] First, 2-aminoterephthalic acid (2.77g) was dissolved in DMF (600ml), and the oil bath was heated to 110°C; then, the AlCl 3 ·6H 2 O (7.24g) was added to the above solution in 8 equal portions (0.905g), AlCl 3 ·6H 2 The mass ratio of O to 2-aminoterephthalic acid is 2.6, and the time interval between adding each equal portion is 15 minutes. After adding the last portion, stir at 110°C for 3 hours, then let stand without stirring for 16 hours, and cool to room temperature; Then, the resulting solid was separated by filtration, washed three times with DMF and ethanol, then stirred and purified in hot ethanol at 90°C for 16 hours, and centrifuged to obtain a yellow solid; finally, vacuum-dried at 120°C for 12 hours to obtain MIL-101-NH 2 .
[0025] The prepared MIL-101-NH 2 (500 mg) was transferred to a ceramic boat and placed in a high-temperature graphite furnace; subsequently, carbonization of the composite was carried out at 900°C for 5 hours under a nitrogen atmos...
Embodiment 2
[0031] First, 2-aminoterephthalic acid (2.77 g) was dissolved in DMF (600 ml), and the oil bath was heated to 110°C; then, AlCl 3 ·6H 2 O (6.37 g) was added to the above solution in 7 equal portions (0.91 g), AlCl 3 ·6H 2 The mass ratio of O to 2-aminoterephthalic acid is 2.3, and the time interval between adding each equal portion is 15 minutes. After adding the last portion, stir at 110°C for 3 hours, then let stand without stirring for 16 hours, and cool to room temperature; Then, the resulting solid was separated by filtration, washed three times with DMF and ethanol, then stirred and purified in hot ethanol at 90°C for 16 hours, and centrifuged to obtain a yellow solid; finally, vacuum-dried at 120°C for 12 hours to obtain MIL-101-NH 2 .
[0032] The prepared MIL-101-NH 2 (500 mg) was transferred to a ceramic boat and placed in a high-temperature graphite furnace; then, under a nitrogen atmosphere (0.1 L / min), the composite was carbonized at 895 °C for 5 hours at a he...
Embodiment 3
[0041] The prepared MIL-101-NH 2 (500 mg) was transferred to a ceramic boat and placed in a high-temperature graphite furnace; subsequently, carbonization of the composite was carried out at 800°C for 5 hours under a nitrogen atmosphere (0.1 L / min), and the heating rate was 5°C / min ; After cooling to room temperature, the carbonized sample was immersed in HF (40% HF: H 2 O = 25ml: 15ml) solution was stirred for 48 hours; then, the black sample was collected by centrifugation and washed several times with a large amount of distilled water; finally, it was dried under vacuum at 120°C for 12 hours to obtain the porous carbon material MNC-800.
[0042] The SEM of the above MNC-800 is as figure 2 (800°C), the irregular texture of the sample deepened. The nitrogen adsorption-desorption curve of MNC-800 was tested by a nitrogen adsorption-desorption instrument, and the BET specific surface area of MNC-800 was 1248 m 2 / g, the total pore volume is 1.032 cm -3 / g, the mesopore v...
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