SUPERCRITICAL EXTRACTION OF ISRAELI MISHOR ROTEM OIL SHALE 1. BATCH EXTRACTION WITH TOLUENE

Publisher Website
Google Scholar
Abstract
Recovery of organic material from Israeli Mishor Rotem oil shale with toluene under supercritical conditions was investigated. The rate of solubilization, change of structural aspects and molecular weights of solubilized products with time were investigated. Experiments to recover organic material from shale were performed in a stainless steel high pressure autoclave. Shale Sample was charged in a sintered glass crucible suspended from the cap of the autoclave; toluene was the solvent in all experiments. Solvent/shale ratio was 20; experimental temperature was 34O°C. The gaseous products were analyzed by gas chromatography. Molecular weights of the organic material recovered was measured by gel permeation chromatography technique. FTIR spectra of the organic material recovered and fractions isolated by extractive and chromatographical methods were measured. The amount of kerogen remaining in the spent shale was determined by oxidative derivative thermal gravimetry. A steady state in the production of solubles was reached within 60 minutes at 340°C with a yield of 60 percent. After this time no further amounts of organic material was recovered. The molecular weights of the recovered organic material decreased at extended times after the steady state was reached. It appeared that the structure of the organic material recovered remained unchanged until the steady state condition is reached whereupon some structural changes occurred. At extended times the organic material was converted into more aromatic and less hydroxyl containing structures of lower molecular weight. The organic material recovered upon reaching steady state was fractionated into 63 percent oils (pentane solubles) and 32 percent asphaltenes (toluene solubles). The oile contained aliphatics and monoaromatic structures and the asphaltenes contained polyaromatic polar structures. Gases which constituted 4 percent of the initial kerogen were produced during the heating period to 340°C. The amount of carbon monoxide produced remained constant and amounts of hydrogen, carbon dioxide and methane decreased after supercritical conditions were attained.