ISSN 1070-4272, Russian Journal of Applied Chemistry, 2007, Vol. 80, No. 3, pp. 448! 455. + Pleiades Publishing, Ltd., 2007.
Original Russian Text + Yu.S. Grushko, V.P. Sedov, V.A. Shilin, 2007, published in Zhurnal Prikladnoi Khimii, 2007, Vol. 80, No. 3, pp. 450 ! 457.
Technology for Manufacture of Pure Fullerenes C
and a Concentrate of Higher Fullerenes
Yu. S. Grushko, V. P. Sedov, and V. A. Shilin
Konstantinov Institute of Nuclear Physics, Russian Academy of Sciences, Gatchina, Leningrad oblast, Russia
Received September 28, 2006; in final form, December 2006
Abstract-An integrated technology for manufacture of fullerenes was developed. It includes the following
stages: synthesis of a fullerene black, extraction of a mixture of fullerenes from the black, preliminary separa-
tion of the mixture into concentrates enriched in C
fullerenes, and production of C
fullerenes of purity exceeding 99.5 and 98.0 wt %, respectively, from the concentrates.
The development of nanotechnologies is a priority
of the XXI century and, beginning in 2000, has been
attracting considerable investment in all the developed
countries of the world. In 2007, the Federal Target
Program [Development of the Infrastructure of Nano-
technologies in the Russian Federation in 200732010]
is brought in force in Russia. According to estimates,
no less than 25% of current nanotechnological designs
are, and will be, associated with use of fullerenes.
However, despite the considerable progress in studies
of fullerenes and development of technologies for
their production, a number of problems have not been
resolved, which hinders wide application of fullerene
nanostructures. The major problem is high cost of
production, separation, and purification of fullerenes.
Several methods for synthesis of fullerenes are
presently known . The most preferable of these
are the electric-arc technique  and method of in-
complete combustion of hydrocarbons (benzene,
toluene, etc.) . Other methods have been poorly
studied and can be only used on a limited scale.
In both methods, the main synthesis product is
the so-called fullerene-containing carbon black (FB).
In addition to fullerenes, the black contains amorph-
ous carbon and, in the case of incomplete combustion
of hydrocarbons, also impurities of polycondensed
A characteristic distinction of fullerenes from other
structures composed of pure carbon is their ability to
dissolve in organic solvents. This enables recovery of
fullerenes from FB by extraction with organic solvents
The integrated technology for manufacture of ful-
lerenes, suggested in this paper, includes stages of FB
synthesis, extraction of a mixture of fullerenes from
the black, and subsequent separation and purification
of the fullerenes (see scheme). This technology has
been used for more than 10 years at the St. Petersburg
Institute of Nuclear Physics for production of kilo-
gram amounts of C
of 99.5% purity (here and here-
inafter, the composition of fullerenes is given in
Manufacture of FB by electric-arc evaporation
of graphite. The fullerene-containing carbon black
produced by the electric-arc method, as a rule, con-
tains a mixture of fullerenes with the following con-
tent of the main components (wt %): C
12330, and C
135. A specific feature of the
electric-arc method is that it produces, together with a
carbon black containing up to 20 wt % fullerenes, also
so-called cathode deposits containing up to 40 wt %
multilayer carbon nanotubes, which a valuable materi-
al for nanotechnologies.
The designs of electric-arc carbon-black generators
(EACBGs), developed by now, provide, under certain
conditions, a fullerene yield of up to 43 wt % .
However, the increase in the fullerene yield entails a
decrease in the evaporation rate of graphite . It has
been noted  that, as the diameter of the electrodes
being evaporated increases, the yield of fullerenes
should necessarily decrease. This circumstance serves
as a certain limitation in developments of a high-
capacity EACBG design [5, 16319].
Processing of FB with low content of fullerenes is
unprofitable because of the increasing expenditure of