We report the development of a novel solvent extraction technique which exploits the coalescence properties exhibited by some solvent combinations at elevated temperatures. The technique allows for instantaneous mixing which approaches the theoretical extraction limit. In the extraction of Pb2+ from aqueous solution into either 2,4-pentanedione or glutaronitrile containing dicyclohexano-18-crown-6 (DC18C6), extraction times were reduced from 2 hours to less than 1 minute. The K-ex value for extracting Pb2+ into glutaronitrile with DC18C6 as the extractant was determined to be 260. The novel coalescence extraction technique is compared to traditional systems in terms of extraction efficiency, speed of extraction, and feasibility of practical applications.