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The escalating levels of carbon dioxide in flue gas and the resultant greenhouse effect have heightened the need for adsorbents with high CO 2 sorption and separation capabilities. However, Traditional heated synthesis methods are energy-intensive and often involve toxic solvents, which are not viable for widespread industrial use. This study introduces a room-temperature, eco-friendly synthesis technique to produce UiO-66-(OH) 2 with varying amounts of PVP (0/0.1/0.2 g), effectively adjusting the particle morphology. Results confirm that this method maintains robust CO 2 adsorption and selectivity. Notably, the addition of 0.1 g of PVP led to a reduction in pore size and adsorption capacity of CO 2 , yet remarkably enhanced its CO 2 /N 2 separation performance sixfold, outperforming traditional CO 2 adsorbents. Dynamic breakthrough experiments further validated the effectiveness of UiO-66-(OH) 2 in separating binary mixtures of CO 2 /N 2 (v/v = 15/85). The separation performance of UiO-66-(OH) 2 on CO 2 /N 2 was significantly improved after the addition of PVP at room temperature. [Display omitted] • OH-functionalized UiO-66 has been successfully synthesized using green room temperature technology. • The addition of PVP can effectively prevent the agglomeration of UiO-66-(OH) 2 , forming dispersed and uniform particles. • UiO-66-(OH) 2 maintains robust CO 2 adsorption and selectivity, which was synthesized at room temperature. • The CO 2 /N 2 separation of UiO-66-(OH) 2 with the addition of PVP increased to 724. [ABSTRACT FROM AUTHOR]