S. Saim et al., SUPERCRITICAL-FLUID EXTRACTION OF FULLERENES C-60 AND C-70 FROM CARBON SOOT, Separation science and technology, 28(8), 1993, pp. 1509-1525
A new branch of organic chemistry has begun to emerge following the de
velopment of a carbon-arc electric discharge process by Kratschmer et
al. which produced a carbon soot containing a series of caged buckmins
terfullerene C60,C70, and higher homologues. While these compounds are
normally recovered either by sublimation in an inert atmosphere or by
extraction with benzene, toluene, or a higher boiling aromatic, enhan
ced selectivity can be achieved by operating at supercritical conditio
ns. The ability of supercritical fluid solvents to fractionate the ext
ractable material of the carbon soot by pressure and/or temperature tu
ning of the solvent power appears to be possible due to the significan
t molecular weight and size difference between C60 and C70 which yield
different threshold solubility densities. While CO2 is unable to extr
act any fullerenes, selective extraction of C60 is obtained when using
a nonaromatic modifier such as cyclopentane. Quantitative recoveries
are achieved by employing moderate concentrations of an aromatic solve
nt modifier such as toluene at pressures imparting solvent densities g
reater than 0.8 g/cm3.