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Characterization of pyrolyzed asphaltenes by diffuse reflectance-Fourier transform infrared and dipolar desphasing-solid state /sup 13/C nuclear magnetic resonance spectroscopy

Conference · · Am. Chem. Soc., Div. Pet. Chem., Prepr.; (United States)
OSTI ID:6482192
The asphaltene fraction is the pentane-insoluble but benzene-soluble portion of the coal liquids. Two coal liquid asphaltenes were used, one from Catalytic Incorporated Solvent Refining Coal (SRC) and one from FMC Char-Oil Energy Development (COED) staged pyrolyses process. The asphaltenes were pyrolyzed slowly under 1 atm of nitrogen to 500/sup 0/C and samples were removed at various temperature intervals. The starting asphaltene, as well as the pyrolyzed asphaltene were subjected to /sup 13/C NMR and Fourier transform ir spectroscopy. Upon pyrolysis, the SRC asphaltene formed a coarse deformed mesophase, and the COED asphaltene formed a fine isotropic mesophase. The aromatic character of both asphaltenes increased with heat treatment temperature, although the transition of the SRC sample was much smoother. Irregularities might be due to cracking and recondensation. The SRC sample is relatively insensitive to heat treatment temperature (HTT), indicating structural transition with temperature is constant. The increase of quaternary to tertiary aromatic carbon types with HTT suggested an increase substitution as well as condensation. Small amounts of ether in COED samples indicate crosslinking of the phenolic hydroxyls, perhaps inhibiting the mesophase growth. 4 figures, 2 tables.
OSTI ID:
6482192
Report Number(s):
CONF-810813-(Vol.2)
Conference Information:
Journal Name: Am. Chem. Soc., Div. Pet. Chem., Prepr.; (United States) Journal Volume: 26:4
Country of Publication:
United States
Language:
English