An experimental apparatus was developed for rapid and continuous supercritical CO2 extraction and separation of hydrophobic organic compounds from liquid solution. The mixing of supercritical CO2 and liquid solutions in a micromixer enhances mass transfer, which enables rapid extraction of hydrophobic organic compounds. Near-equilibrium yields were obtained in about 10 s. The separation of supercritical CO2 from liquid was achieved using a newly developed separation system. In this separation system, the liquid level is controlled by the differential pressure between the head pressure and the supercritical CO2 phase. A control bulb at the outlet of the liquid line was regulated to maintain a constant differential pressure. The extraction of aqueous vanillin solution was conducted at 40 degrees C under pressures of 10, 15, and 20 MPa. Our results suggest that greater than 97% equilibrium was achieved in our system within the extraction time of 10 s. The extraction of a black liquor filtrate, that contains vanillin, its related compounds, and more than 5 wt % salts, was also conducted. More than 80% of the vanillin was successfully extracted to the CO2 phase.