Method for large-scale preparation of high-crystallization high-specific-surface-area covalent triazine framework
A high specific surface area, covalent triazine technology, applied in the application field of antibiotic adsorption, can solve the problems of unclear mechanism, high monomer price, unsuitable for large-scale preparation and industrial application, etc., and achieves simple operation process, excellent Antibiotic adsorption performance, the effect of easy large-scale preparation
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Embodiment 1
[0032] Mix the monomer 1,4-dicyanobenzene (DCB) (125mg) and the catalyst polyphosphoric acid (879mg) into a 10ml quartz heat-resistant tube, cool in liquid nitrogen, melt and seal it, and transfer it to a muffle furnace . The temperature programming process of the muffle furnace is: heating at 100°C for 2h, heating at 180°C for 2h, heating at 260°C for 2h, heating at 340°C for 2h, and finally heating at 400°C for 8h, and the heating rate of each step is 2°C / min. After the reaction, the sealed tube was cooled to room temperature and opened, washed sequentially with ammonia water, ethanol, acetone and tetrahydrofuran, and vacuum-dried at 120°C for 24 hours to obtain the crystalline product CTF-DCB with a yield of 73%.
Embodiment 2
[0034] Mix the monomer 1,4-dicyanobenzene (DCB) (250mg) and the catalyst polyphosphoric acid (879mg) into a 10ml quartz heat-resistant tube, cool in liquid nitrogen, melt and seal it, and transfer it to a muffle furnace . The temperature programming process of the muffle furnace is: heating at 100°C for 2h, heating at 180°C for 2h, heating at 260°C for 2h, heating at 340°C for 2h, and finally heating at 400°C for 8h, and the heating rate of each step is 2°C / min. After the reaction, the sealed tube was cooled to room temperature and opened, washed sequentially with ammonia water, ethanol, acetone and tetrahydrofuran, and dried in vacuum at 120°C for 24 hours to obtain the crystalline product CTF-DCB. The nitrogen content was 14.15% as determined by elemental analysis, and the yield was 85%. The prepared crystalline product CTF-DCB has high crystallinity and matches well with the theoretically simulated AA packing model, as shown in figure 2 (a) shown. Its nitrogen adsorptio...
Embodiment 3
[0036] Mix the monomer 1,4-dicyanobenzene (DCB) (500mg) and the catalyst polyphosphoric acid (879mg) into a 10ml quartz heat-resistant tube, cool in liquid nitrogen, melt and seal it, and transfer it to a muffle furnace . The temperature programming process of the muffle furnace is: heating at 100°C for 2h, heating at 180°C for 2h, heating at 260°C for 2h, heating at 340°C for 2h, and finally heating at 400°C for 8h, and the heating rate of each step is 2°C / min. After the reaction, the sealed tube was cooled to room temperature and opened, washed successively with ammonia water, ethanol, acetone and tetrahydrofuran, and vacuum-dried at 120°C for 24 hours to obtain the crystalline product CTF-DCB with a yield of 72%. The comparison picture of 2 is as follows Figure 4 shown.
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