An alternative method for using monoethanolamine (MEA) in CO2 separation is developed from the viewpoints of the MEA-CO2 reaction environment and the process of spent sorbent regeneration. The method could be used to considerably reduce energy consumption compared to conventional aqueous MEA processes. MEA-TiO2 (MT) CO2 sorbent is synthesized using pure MEA and a support material, TiO2. The performance of the MT sorbent on CO2 separation was investigated in tubular reactors under various experimental conditions. The effects of several major factors on CO2 sorption by the MT sorbent were investigated. The sorption capacity of the MT sorbent increased with MEA loading, reaching 48.1 mg-CO2/g-MT at 45 wt% MEA. However, an optimum of 40 wt% MEA loading was chosen for most of the sorption tests conducted in this research. Temperature affected the CO2 sorption capacity considerably, with optimum values of 45°C for adsorption and 90°C for regeneration, while humidity had a small positive effect under initial test conditions. In addition to TiO2, TiO(OH)2 and FeOOH were also tested as potential supports for MEA. TiO(OH)2 appears to be the best support material for MEA, but more evaluation is needed. The MT sorbent is regenerable, with a multi-cycle sorption capacity of ~40 mg-CO2/g-MT under the given experimental conditions.