Supercritical fluid extraction was evaluated for removing surfactants from freshly synthesized molecular sieve powders possessing different pore sizes. In our study, methanol- or water-enhanced supercritical CO2 extraction was carried out on as-synthesized microporous and mesoporous material powders. The results showed that very high surfactant recovery (over 80%) could be achieved from large pore-sized mesoporous materials by using the SFE method, while the surfactant recovery is rather low from small pore-sized microporous zeolite materials. Supercritical fluid extraction technology may provide a potential method for large-scale production of mesoporous materials with effective surfactant recovery that is extremely efficient. (c) 2004 Elsevier B.V. All rights reserved.