PARTICLE SIZE, SOLVENT, OXYGEN, TEMPERATURE AND PRESSURE EFFECTS ON THE CONTENTS OF INSOLUBLE FRACTIONS FROM SOLID VACUUM RESIDUA

n-Heptane insoluble contents were determined for an extraheavy-oil vacuum residue, one petroleum and one coal pitch as a function of particle size. This variable was found to affect the yields of insoluble material, aspect which was also observed during extractions carried out with aromatic and halogenated solvents. The precision of results was observed to be independent on the operators. A study was carried out to determine the effect of sample drying time on fraction yields. It was found that maltene fractions were strongly dependent on this variable, whereas asphaltene fractions were totally independent

Predissolution in aromatic solvents proved worthless from the repeatability point of view. However, predissolution of the oil residue in CH₂Cl₂ followed by filtration and asphaltene precipitation with simultaneous solvent removal, was deemed to be a suitable technique to remove mineral matter and isolate asphaltenes in a single step

Sample oxidation during asphaltene precipitation and isolation was detected by gravimetric and spectroscopic techniques. This fact is very important since common precipitation techniques do not address this issue

Preliminary accelerated extraction experiments carried out with pitch samples at high temperature and pressure, revealed that this approach can be a very interesting research tool to investigate solubility properties.     

PARTICLE SIZE,SOLVENT, OXYGEN,TEMPERATURE AND PRESSURE EFFECTS ON THE CONTENTS OF INSOLUBLE FRACTIONS FROM SOLID VACUUM RESIDUA

ABSTRACT

n-Heptane insoluble contents were determined for an extraheavy-oil vacuum residue, one petroleum and one coal pitch as a function of particle size. This variable was found to affect the yields of insoluble material, aspect which was also observed during extractions carried out with aromatic and halogenated solvents. The precision of results was observed to be independent on the operators. A study was carried out to determine the effect of sample drying time on fraction yields. It was found that maltene fractions were strongly dependent on this variable, whereas asphaltene fractions were totally independent

Predissolution in aromatic solvents proved worthless from the repeatability point of view. However, predissolution of the oil residue in CH₂Cl₂ followed by filtration and asphaltene precipitation with simultaneous solvent removal, was deemed to be a suitable technique to remove mineral matter and isolate asphaltenes in a single step

Sample oxidation during asphaltene precipitation and isolation was detected by gravimetric and spectroscopic techniques. This fact is very important since common precipitation techniques do not address this issue

Preliminary accelerated extraction experiments carried out with pitch samples at high temperature and pressure, revealed that this approach can be a very interesting research tool to investigate solubility properties.