In this study, a low-temperature coal tar pitch (CTP1) was subjected to carbonization in order to study the formation, growth, and development of mesophase achieved under different conditions. The results were compared to those obtained with a petroleum pitch (PP) and a conventional high-temperature coal tar pitch (CTP2). CTP1 was converted to mesophase at a considerably lower temperature, and also mesophase develops and coalesces at a markedly higher rate for this pitch. Volatile matter removal is a key factor in mesophase formation, but chemical composition also plays an important role, with substituted cata-condensed compounds constituting very reactive components in terms of anisotropic material development. More specifically, the oxygenated functional groups and aliphatic substituents facilitate the growth of mesophase. In particular, the high concentration of phenolic compounds present in CTP1 seems to contribute to the fast coalescence of mesophase spheres. The effect of several additives was also studied. Ferrocene was the most efficient in terms of mesophase formation, but simultaneously inhibiting coalescence. In contrast the use of argon pressure during carbonization promotes contact between mesophase spheres.
Several chromatographic procedures were developed by the
authors for the structural
characterization and fractionation of pitches. Six coal tar
pitches obtained by heat treatment
under different conditions, together with a typical mesophase petroleum
pitch, chosen for
comparison, were studied following these procedures. The results
gave an insight into the kind
and extension of the chemical transformation occurring in pitch
structure as a consequence of
heat treatment. A good LC fractionation in compound classes
(confirmed by FT-IR and HPLC
analyses) of the toluene-soluble materials was achieved. The
thermal behavior of the pitches
was studied by thermogravimetric analysis and differential
thermogravimetry, establishing a
correlation between the softening point and the temperature of maximum
weight loss rate. When
toluene-soluble fractions are considered, HPLC and LC results indicate
that the increasing heat
treatment temperature gives rise to a decrease in the content of
unsubstituted planar cata-condensed compounds, with a corresponding increase in the
peri-condensed compounds concentration and a general increase in the condensation degree of polyaromatic
structures. The distillation
of the parent tar, followed to obtain the soft coal tar pitch CTSP,
promotes an extensive removal
of alkyl- and aryl-substituted aromatic compounds which are
subsequently present in small
quantities in all the studied pitches. Petroleum pitch PP consists
of a high proportion of
substituted cata-condensed compounds while coal tar pitch
CTP-2, with similar SP and QI content,
contains peri-condensed compounds and β-resins as its main
components.
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