Investigation of the Thermal Behavior and Interaction of
Venezuelan Heavy Oil Fractions Obtained by
Ion-Exchange Chromatography
Parviz Rahimi* and Thomas Gentzis
National Centre for Upgrading Technology, 1 Oil Patch Drive, Suite A202, Devon,
Alberta T9G 1A8, Canada
Edgar Cotte ´
PDVSA, Intevep, Caracas 1070A, Venezuela
Received October 11, 1998. Revised Manuscript Received January 2, 1999
The coking propensity of Hamaca heavy oil (+510 °C) and its fractions separated by
ion-exchange chromatography was investigated using hot-stage microscopy. The initial time of
mesophase formation and its growth rate were measured for each fraction. The results showed
that the amphoteric fraction was the most prone to coke formation, followed by the basic and
acidic fractions. Mesophase formation for the neutral and aromatic fractions was delayed, and
its growth rate was considerably slower. The relative order of coking propensity of the fractions
is amphoteres > bases > Hamaca resid > acids > neutrals > aromatics. Although the Hamaca
resid contained high concentrations of aromatic and neutral components with a relatively lower
coking propensity, its coking propensity was much more similar to that of the acidic and basic
fractions, which were less abundant in the resid. This propensity shows that the interactions
among the individual components were not proportional to their concentrations in the feed and
that the amphoteric fraction may have had a larger influence on coke formation relative to the
other components. It was further observed that under the reaction conditions employed, the
amphoteric fraction had high viscosity, did not develop a distinct mesophase stage, and formed
fine-grained mosaic coke over a very short period of time. The results of this work may be used
to assess the feasibility of selective removal of problematic components in the feedstocks prior to
processing.
Introduction
Predicting the product yields and quality during the
hydrocracking of heavy oils is challenging because of
the complexity of the cracking reactions and the vari-
ability in the chemical composition of the feedstocks.
The use of analytical techniques that provide not only
consistent and meaningful results, but also sufficient
quantities of resid fractions for further evaluation and
analyses is crucial. Petroleum fractions can be obtained
using techniques such as distillation, SARA, liquid
chromatography (LC), supercritical fluid extraction
(SCFE), and ion-exchange chromatography (IEC). Fur-
thermore, the relationships between the chemical com-
position of the feedstocks and the products are well
established. For instance, the yields of gas, gasoline,
light gas oil (LGO), and heavy gas oil (HGO) and
amount of coke that result from fluid catalytic cracking
(FCC) of the Californian Wilmington resid were shown
to depend on feedstock composition.
1
There is evidence
that the majority of the light products, such as gas and
gasoline, are derived primarily from the neutral com-
ponents of the feed. Large amounts of coke and small
quantities of methane and C
2+
hydrocarbons that form
during the processing of petroleum heavy ends are
attributed to the acidic and basic components in the
feed. It has also been shown that the polar compounds
present in acidic and basic fractions not only influence
the storage stability and utilization of distillates but also
play a key role in sediment formation in diesel fuels.
2,3
Ovalles et al.
4
studied the thermal stability and
interfacial activity of acid, basic, and neutral fractions
in the Cerro Negro Crude Oil from Venezuela, obtained
by the IEC method. Following characterization of the
fractions via spectroscopic techniques (FTIR, H and
13
C
NMR), they concluded that acid fractions behaved as
natural surfactants in stabilizing oil/water emulsions
and that it was the hydrophilic portion of the surfac-
tants that showed higher acidity and high concentration
of polar constituents. Acid fractions are known to be
responsible for coke formation,
5
to deactivate heteroge-
neous catalysts in day-to-day operations of refineries,
* To whom correspondence should be addressed.
(1) Green, J. B.; Zagula, E. J.; Reynolds, J. W.; Wandke, H. H.;
Young, L. L.; Chew, H. Energy Fuels 1994, 8, 856-867.
(2) Pedley, J. F.; Hiley, R. W.; Hancock, R. A. Fuel 1988, 67, 1124-
1130.
(3) Pedley, J. F.; Hiley, R. W.; Hancock, R. A. Fuel 1989, 68, 27-
31.
(4) Ovalles, C.; del Carmen Garcia, M.; Lujano, E.; Aular, W.;
Bermudez, R.; Cotte ´, E. Fuel 1998, 77, 121-126.
694 Energy & Fuels 1999, 13, 694-701
10.1021/ef980220m CCC: $18.00 © 1999 American Chemical Society
Published on Web 03/04/1999