A new technique to prepare adsorbent for CO2 capture was applied in this study. Silica was selected to be support as the adsorbent and Tetraethenylpentamine (TEPA) was syringed on it to be the sorbent. It allowed a sample to be in few minutes and also presented well performance. A relatively lower regeneration temperature was be used in this study to renew the adsorbent. In this study, by observation of in situ infrared (IR) spectra and temperature programmed desorption (TPD), CO2 was found to adsorb each other in multiple layers through hydrogen bonding. In present water environment, substantial spacial barrier produce to effect CO2 adsorption. On the aspect of competitive adsorption between CO2 and water is also study by IR spectra, which CO2 adsorbed on TEPA-treated silica earlier than water.