Mineral matter effects and catalyst characterization in coal liquefaction. Second quarterly report. January--March 1978

Coal liquefaction experiments were carried out in an autoclave facility modified for the rapid (approximately 5 sec) addition of a coal/solvent slurry into a preheated solvent. Sixteen slurry addition experiments have been completed with Illinois No. 6 coal in tetralin solvent. Six runs were carried at 408/sup 0/C, 1500 psig and a solvent-to-coal ratio of 4.0, in order to evaluate the effects of residence time (2, 10 and 40 min) and mineral additions (20 wt percent THF-extracted filter cake) on coal liquefaction. Conversion to benzene solubles increased from 24 to 60 percent as residence time increased from 2 to 40 min. An additional 1 to 4 percent increase in conversion occurred when mineral matter was added to the feed slurry. The preasphaltenes increased from 35 to 38 percent, and then decreased to 29 percent as residence time increased from 2 to 40 min. Additional increases in preasphaltenes occurred in the presence of added mineral matter. Hydrogen consumption increased from 0.5 to 1.4 percent as residence time increased. Three fresh and two spent catalysts from the bench reactor at Hydrocarbon Research, Inc. were received. A test matrix has been developed for the quantitative analysis of Co, Ni, Mo, Fe, Ti, Mg,more » Ca, Zn, Na, Al, Si, and S by electron microprobe analysis, emission spectroscopy and atomic absorption spectroscopy. The electron microprobe will be used for an elemental mapping of approximately 10 percent of the cross sectional area of a catalyst sample. Preliminary data have shown that Ti increased from approximately 2 percent on the surface of a spent catalyst to approximately 7 to 8 percent at 50 to 100 ..mu..m depth, and then decreased to approximately 2 percent at 200 ..mu..m.« less