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Identification and cleavage of breakable single bonds by selective oxidation, reduction, and hydrolysis. Quarterly report No. 10, January 1-March 31, 1981

Technical Report ·
OSTI ID:6290889

The objective is to determine the structure of coal with emphasis on the crosslinks and breakable single bonds. Near the end of the first year, we found that benzylamine (BnNH/sub 2/) would extract an additional 14% (of the original weight of coal) of material from pyridine-extracted coal. More recently, we found that an EDA-DMSO (ethylene diamine-dimethyl sulfoxide) mixture would dissolve an additional 19% of the original coal. The BnHN/sub 2/ extract is nearly wholly soluble in pyridine, but the EDA-DMSO extract is only partly soluble in pyridine. Our best present guess is that the BnNH/sub 2/ cleaves most of the ester groups in coal and that EDA-DMSO cleaves the remaining ester and most of the ether groups, thus liberating additional material from the pyridine-insoluble coal network. These two extracts are interesting for structural studies because they were part of the pyridine-insoluble portion of whole coal, instead of being unattached accompanying material. The EDA-DMSO-extracted coal is of interest for investigating connecting links, because it represents a smaller proportion of the coal network, perhaps containing only hydrocarbon connecting links. The experimental section of this report describes: solubilities of the EDA-DMSO extracts of Illinois No. 6 coal and the treatment of an extract with sodium; last details (Cl analysis) of an earlier treatment of EDA-DMSO-extracted coal with zinc chloride; oxidations of extracted coals with nitric acid, formic acid + hydrogen peroxide, and oxygen + t-BuOK in pyridine; recent efforts to characterize various oxidation products, mostly black acids; and shows that sulfolane extracted only 0.7% of whole Illinois No. 6 coal. 3 figures, 3 tables.

Research Organization:
SRI International, Menlo Park, CA (USA)
DOE Contract Number:
AC22-78ET11423
OSTI ID:
6290889
Report Number(s):
DOE/ET/11423-T16; ON: DE85003860
Country of Publication:
United States
Language:
English