Executive SummaryTo provide a better understanding of the roles of a solid catalyst and the solvent in Direct Coal Liquefaction, a small reactor was equipped with a porous-walled basket which was permeable to the solvent but was not permeable to the cod or solid catalyst.With this equipment and a high volatile bituminous coal it was found that direct contact between the catalyst in the basket and the coal outside the basket is not required for catalyzed coal liquefaction. The character of the solvent in this system makes a significant difference in the conversion of the coal, the better solvents being strong donor solvents.Because of the extensive use of thermogravimetric analysis in this laboratory, it was noted that the peak temperature for volatiles evolution from coal was a reliable measure of coal rank. Because of this observation, a variety of coals of a range of ranks was investigated. It was shown in this work that measuring the peak temperature for volatiles evolution was a quite precise indicator of rank and correlated closely with the rank value obtained by measuring vitrirlite reflectance, a more difficuit measurement to make.This prompted the desire to know the composition of the volatile material evolved as a function of coal rank. This was then measured by coupling a TGA to a mass spectrometer using laser activation and photoionization detection TG-PI-MS. The predominant species in volatiles of low rank coal turned out to be phenols with some alkenes. As the rank increases. the relative amounts of alkene and aromatic hydrocarbons increases and the oxyge actually pyrolytic products and not volatilization products of the cod. d species decrease. It was shown that se volatiles were Solvent extraction experiments coupled with Thennogravimetric-photoionizationmass sp+ctrometry (TG-PI-MS) indicated that the low boiling and more extractable material w essentially similar in chemical types to the non-extractable portions but apparently higher molecular weight and therefore less extractable.
IntroductionDespite many years of research on Direct Coal Liquefaction, there are still some aspects of the process which are not fully understood and yet could have important implications for process improvement. Among these questions are the roles of the solid catalyst and the solvent. Seavel(1) showed that hydroaromatic solvents in direct liquefaction in the absence of a catalyst act primarily as a donor of hydrogen atoms to the free radicals formed as the coal is broken down thermally under coal liquefaction conditions. This minimizes degradative reactions of these radicals which otherwise form insoluble and unreactive products. Much emphasis in modem coal liquefaction studies however has been on liquefaction in the presence of both a donor solvent and a solid catalyst such as nickeUmoiybdenum or cobaitlmolybdenum on an alumina support.Tomlison (2) and others (3.4) have shown that adding a solid catalyst'in coal liquefaction produced higher conversion and oil yields of higher quality. Weller and Pelipetz ( 5 ) als...