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U.S. Department of Energy
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Physical and chemical behavior of liquefied coal in solids separation. Quarterly report, April-June 1979

Technical Report ·
OSTI ID:5757448
A technique was perfected for precipitating organic bases from THF solutions with phosphotungstic and phosphomolybdic acids. The procedure can be used to isolate the basic fraction of preasphaltenes. Nitrogen heterocycles can be removed from Deno oxidation products by formation and precipitation of the Reineckate salt of aromatic amines from aqueous acid solutions. The procedure was used to remove the heterocycles prior to esterification. BF/sub 3/ catalyzed esterification gave reproducible results on several coal derived liquids. The compressibility of filter cake produced from the filtration of H-Coal product oil was 1.14 compared to 0.55 when Soltrol 130 is added to give a slurry concentration of 20 wt % Soltrol 130 prior to filtration at 232/sup 0/C. Small angle x-ray scattering experiments with GPC fractionated asphaltene samples indicate that the colloidal state of the asphaltene solution depends upon the nature of the homogeneous phase. For a high heteroatom content fraction in pyridine at 10 wt %, the micelles exist as a nominally monodisperse system with a radius of gyration of 14.8 A. In a mixture of 90 wt % tetralin, 2.5 wt % m-cresol and 7.5 wt % ..cap alpha..-picoline at a concentration of 10 wt %, the same fraction is a polydisperse system with 98.5 of the micelles having a radius of gyration of 6.61 A and 1.50 wt % having a radius of gyration of 41.8 A or greater. An oil and resin fraction from the liquefaction of an Illinois No. 6 coal in the H-Coal process was subjected to oscillatory testing with the Weissenberg rheogoniometer to determine the viscoelastic properties of the fraction.
Research Organization:
Michigan Univ., Ann Arbor (USA). Dept. of Chemical Engineering
DOE Contract Number:
AS01-76ET10550
OSTI ID:
5757448
Report Number(s):
DOE/ET/10550-T3; FE-2550-11; ON: DE82004541
Country of Publication:
United States
Language:
English