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Novel MgO/hollow carbon sphere composites for CO2 adsorption have been synthesized through a one-pot self-assembly approach followed by carbonization. The interaction between the carboxyl groups of precursors and Mg2+ benefits a high dispersion of MgO based species over the carbon support, inducing an enhanced CO2 uptake capacity up to 122.96 mg g−1 at 25 °C and 1 bar. The uniform distribution of MgO and the interaction between MgO and the carbon support suppresses the aggregation of MgO, and leads to a good recyclability. [ABSTRACT FROM AUTHOR]