Hybrid Two-step synthesis method for preparation of MgAl LDHs materials for CO 2 adsorption has been employed because of the features of fast micromixing and enhanced mass transfer by using a 'T-mixer' reactor. MgAl LDHs with different morphologies were successfully obtained by three different synthesis routes: ultrasonication-intensified in 'T-mixer' (TU-LDHs), conventional co-precipitation (CC-LDHs) and ultrasonic-intensified in 'T-mixer' pretreatment followed by conventional co-precipitation (TUC-LDHs). The synthesized samples characterized by the XRD showed that LDHs formed a typical layered double hydroxide structure and no other impurities were identified in the compound. The SEM and TEM analyses also confirmed that the size distribution of TUC-LDHs was relatively uniform (with an average size of approximate 100 nm) and layered structure was clearly visible. The BET characterization indicated that such LDHs had a large surface area (235 m 2 g À1 ), which makes it a promising adsorbent material for CO 2 capture in practical application. It can be found that the CO 2 adsorption capacities of TU-LDHs, CC-LDHs and TUC-LDHs at 80°C were 0.30, 0.22 and 0.28 mmol g À1 , respectively. The CO 2 adsorption capacities of TU-LDHs, CC-LDHs and TUC-LDHs at 200°C were 0.33, 0.25 and 0.36 mmol g À1 , respectively. The order of CO 2 adsorption capacity to reach equilibrium at 80°C seen in Avrami model is: TU-LDHs > TUC-LDHs > CC-LDHs. The CO 2 adsorption/desorption cycling test reveals that TU-LDHs and TUC-LDHs have good adsorption stability than CC-LDHs.