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Identification and cleavage of breakable single bonds by selective oxidation, reduction, and hydrolysis

Technical Report ·
OSTI ID:5383773

The objective of this project is to determine the proportions of the various kinds of connecting links in coal and how they can best be broken - in other words, to determine the structure of bituminous coal, with emphasis on the cross-links and breakable single bonds. An extraction of Illinois No. 6 coal, some swelling experiments on Illinois No. 6 coal products, and some extractions of other recently acquired coal samples are described. The results show that on long heating at a high solvent-to-coal ratio ethanolamine does not extract as much material from whole coal as either BnNH/sub 2/ or EDA, yet the swelling ratio of the extracted coal is greater than with the other amines. BnNH/sub 2/ swells both EDA/DMSO- and pyridine-extracted coals better than other amine solvents tested, including ethanolamine. The EDA/DMSO-extracted coal is swollen more by all the solvents tested than pyridine-extracted coal. Preliminary results show that solvents swell EDA/DMSO-extracted coal more when either t-BuOK or tetraalkylammonium hydroxides are added to the solvents than when the pure solvents are used but are not conclusive. Results from pyridine extractions of several coals of varying ranks show that less coal is extracted by pyridine as the coal rank increases. A series of oxidations with nitric acid and sodium hypochlorite are described. Model compounds are being oxidized to determine the best way to distinguish between single and multiple methylene groups. Results from ESR measurements on a pyridine extraction of Illinois No. 6 coal are reported. Most of the free spins remain in the insoluble fractions and 38 +- 7% of the spins are lost during the extraction.

Research Organization:
SRI International, Menlo Park, CA (USA)
DOE Contract Number:
AC22-78ET11423
OSTI ID:
5383773
Report Number(s):
DOE/ET/11423-T4; ON: DE82016800
Country of Publication:
United States
Language:
English