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Microporous carbon has been widely known as a probable material to capture greenhouse gases. This work provides a facile synthesis of monodisperse biomass-derived microporous carbon spheres (CSs) for effective CO 2 capture. The spheres were synthesized by a novel continuous microfluidic strategy from oil-inwater-in-oil ((O 1 /W 2 )/O 2 ) emulsions. O 1 nanodroplets could be self-assembled into the cores of micelles, which were formed by chitosan and surfactant F127 in the W 2 phase through high-speed liquid-phase shearing. The obtained O 1 /W 2 emulsion can be further sheared into a sphere by the O 2 phase. After carbonization, nanodroplet-templated pores shrank to micropores and ultramicropores. The optimal sample showed the developed pore structure with a Brunauer−Emmett−Teller (BET) surface area of 576 m 2 /g and microporous volume of 0.22 cm 3 /g. Compared with O 1 free CS, the dynamic adsorption capacity of CO 2 was improved to 1.20 mmol/g from 0.42 mmol/g. The CO 2 capture capacity, cycling stability, isosteric heats, and mass diffusion coefficient of CSs were evaluated as well. The results demonstrate that microporous CSs are promising candidates for CO 2 capture with low cost and a green synthesis route, which was achieved via continuous microfluidic strategy using sustainable biomass chitosan as a carbon precursor and droplets as templates.

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