Reactivity of Heteratom-Containing Organics During Liquefaction of Subbituminous Coal: Quarterly Technical Progress Report, December 15, 1987-March 15, 1988

摘要

The objective of this research project is to provide a greater understanding of the role of heteroatom-containing species in coal reactivity during liquefaction. Work focused on devising and refining a method for synthesizing 1.0 gram quantities of deuterium-labeled 'tracer' species to be used in upcoming liquefaction tests. Rather than performing the reactions in stainless steel tubing bombs which would have to be disposed of after one use due to chloride ion corrosion, glass reactors were designed and fabricated. To equalize pressures inside and outside the glass reactor during the reaction at 300 degrees C, the reactor was placed in a Parr bomb containing an appropriate amount of water. Optimization of conditions included determining the amount of water needed in the Parr bomb to prevent bursting the glass reactors. These tests were conducted using sealed reactors containing only water, instead of reactant species and hydrochloric acid. Following testing, 1.0 gram quantities of nine compounds were deterium-labeled to at least 95% isotopic purity, including phenol, paracresol, guaicol, dibenzofuran, dibenzothiophene, quinoline, methylfluorene, dihydrophenanthrene, and dihydroanthracene. All species listed except dihydrophenanthrene and dihydroanthracene (which will be used to monitor hydrogen shuttling activity) have been identified in liquefaction products. The main advantage in using glass instead of stainless steel to contain the deuteration reaction is that the conditions needed for a successful reaction in glass are known. (ERA citation 13:032075)