Dissolution of the Argonne Premium Coal Samples in strong base
The objective of this study is to solubilize the Argoruie Premium Coal Samples in order to facilitate analysis by mass spectrometry, FTIR and NMR. Earlier, in a search for relatively mild methods for solubilizing coal, we discovered that treating coals with potassium hydroxide in ethylene glycol at 250{degrees}C to be quite an effective approach. Under these conditions, secondary reactions which may obscure the distribution of the basic building blocks of the coal structure are not expected to occur. At higher temperatures, such as those used in more traditional liquefaction processes ({gt} 400{degrees}C), secondary reactions such as the formation of polycyclic aromatic and heteroaromatic compounds dominate. A focus of our approach to characterization of coals is desorption-pyrolysis high resolution CI and EI mass spectrometry and laser desorption mass spectrpmetry (LDMS). It has been shown by PyMS that the yields and the distribution of products is superior for coal extracts compared to the original whole coals. There appears tobe few secondary reactions occurring and many molecules, which are released in analysis of the extract, are trapped in the solid matrix of the coal and never observed. In addition, soluble materials are more amenable to LDMS. The glycol/KOH system was chosen since in early work up to 93% of the product was soluble for lower-rank bituminous coals. Others have solubilized coals under basic conditions. Ouchi and co-workers used ethanolic - NaOH at temperatures ranging from 260{degrees}C to 450{degrees}C. More recently, Stock and coworkers have discussed the use of Lochmann`s base (potassium tert-butoxide, n-butyl lithium in heptane at reflux) which is especially effective for the higher rank coals. Also, a base hydrolysis is included in a low severity liquefaction scheme devised by Shabtai and coworkers.
- Research Organization:
- Argonne National Lab., IL (United States)
- Sponsoring Organization:
- USDOE, Washington, DC (United States)
- DOE Contract Number:
- W-31109-ENG-38
- OSTI ID:
- 10136085
- Report Number(s):
- ANL/CHM/CP-78107; CONF-930304-7; ON: DE93008661
- Resource Relation:
- Conference: 205. American Chemical Society national meeting,Denver, CO (United States),28 Mar - 2 Apr 1993; Other Information: PBD: [1993]
- Country of Publication:
- United States
- Language:
- English
Similar Records
Studies of coupled chemical and catalytic coal conversion methods. Ninth quarterly report, October, November, December 1989
Studies of coupled chemical and catalytic coal conversion methods