The rising demand for sustainable energy storage and carbon mitigation calls for multifunctional materials that integrate high surface area, tailored heteroatom chemistry, and robust electrochemical stability. Herein, we report a continuous three-step synthesis of two novel heterocyclic Schiff base–derived benzoxazine monomers—3-(6-methoxybenzo [d]thiazol-2-yl)-3,4-dihydro-2H-benzo[e][1,3]oxazine (SA-tz Bz) and 3-(6-methoxybenzo [d]thiazol-2-yl)-3,4-dihydro-2H-naphtho[2,1-e][1,3]oxazine (NA-tz Bz)—through sequential Schiff base formation, reduction, and Mannich condensation. Thermal ring-opening polymerization followed by direct carbonization at 600 and 700 °C under an inert atmosphere yielded N, O, S co-doped microporous carbons (C@poly (SA-tz Bz) and C@poly (NA-tz Bz)) without the need for activating agents or wastewater generation. These heteroatom-enriched carbons exhibit disordered amorphous structures with hierarchical porosity, abundant pyridinic/pyrrolic nitrogen species, and oxygen/sulfur functionalities, as confirmed by BET, Raman, XPS, and TEM analyses. Electrochemical studies revealed that C@poly (NA-tz Bz 700) delivers a high specific capacitance of 423 ± 18 F g−1 at 0.5 A g−1 in a three-electrode system, good cycling stability (98 % retention after 6000 cycles), and superior performance in a symmetric two-electrode device (342 F g−1, 89.50 % retention after 4000 cycles). Moreover, C@poly (NA-tz Bz 700) achieves an exceptional CO2 adsorption capacity of 231.7 cm3 g−1 at 273 K, surpassing many reported heteroatom-doped carbons. This work presents a sustainable strategy for designing heterocyclic benzoxazine-derived microporous carbons that combine efficient energy storage with effective CO2 capture, offering promising prospects for next-generation electrochemical and environmental applications.
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