Solvent Analysis of Coal-Derived Products Using Pressure Filtration

Utz, Bruce R.; Narain, Nand K.; Appell, H.R.; Blaustein, Bernard D.

doi:10.1021/bk-1982-0205.ch011

Cited by 4 publications

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“…Representative samples of the feedstocks and products from each run were collected and subjected to detailed analyses. The feedstocks and products were separated via a pressure filtration technique ( Utz et al, 1982) using either cyclohexane or pentane in order to determine the concentration of the "asphaltenes" present in the sample. Each feedstock and product sample was also separated into three fractions (i.e., <616K, 616K to 728K, >728K) using a B/R Instrument Model 24T spinning-band vacuum-distillation unit.…”

Section: Methodsmentioning

confidence: 99%

Noncatalytic conversion of residuum in two‐stage coal liquefaction

Stiegel¹,

Lett²,

Cillo³

et al. 1987

Can J Chem Eng

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An experimental investigation was conducted to ascertain the contribution of thermal reactions in the hydroprocessing reactor of two‐stage liquefaction processes. Various solvent/residuum feedstocks were reacted in the absence of a catalyst at temperatures ranging from 655K to 728K. Detailed characterization of the composite and fractionated feedstock and product samples was performed to ascertain the extent of residuum conversion, heteroatom removal, and hydrogen rearrangement. The results showed that hydrogenation of the solvent portion of the feedstock neither enhances residuum conversion nor results in the transfer of hydrogen from the solvent to the residuum. Higher reaction temperatures also had little effect on the reactions involved. These results suggest that the conversion of residuum in the hydroprocessing reactor of two‐stage liquefaction processes must occur catalytically rather than thermally.

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Section: Methodsmentioning

confidence: 99%

Noncatalytic conversion of residuum in two‐stage coal liquefaction

Stiegel¹,

Lett²,

Cillo³

et al. 1987

Can J Chem Eng

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“…The combined THF extract was filtered through a 5-µ Teflon filter by a pressure filtration apparatus. The details of this procedure are described elsewhere (Utz et al, 1982). The THF-insoluble residue was washed with additional THF, using a total volume of 1000 mL of THF.…”

Section: Methodsmentioning

confidence: 99%

Effect of temperature, coal, donor solvent, and hydrogen on short contact time liquefaction yields

Narain¹

1985

Ind. Eng. Chem. Prod. Res. Dev.

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Ind. Eng. Chem. Prod. Res. Dev. 1985, 2 4 , 641-644 641 noted above, a total yield of single-ring phenols and hydrocarbons of 9.6 w t % would be calculated. This figure compares favorably with the total single-ring phenols' and hydrocarbon yields of less than 2 wt % obtained from pyrolysis alone. Conclusions 1. Preferred products from the hydrodeoxygenation of substituted guaiacols and catechols at temperatures of 250-325 "C were predominantly alkylated phenols and single-ring hydrocarbons, with combined molar yields of up to 0.60 observed. Conversion of these substrates to char was greatly reduced in comparison to pyrolysis alone.2. Hydrocracking of thermally stable biphenyl, diphenylmethane, and phenyl ether interaromatic unit linkages was achieved at temperatures of 280-330 OC during the hydrodeoxygenation of o,o'-biphenol, ohydroxydiphenylmethane, and phenyl ether substrates. Oxygen removal prior to interunit bond cleavage was also observed.3. These model compound results were applied to liquefaction of actual lignins. A 5-fold increase, relative to pyrolysis, in the total yield of single-ring phenols and hydrocarbons was predicted to occur from catalytic liquefaction at milder conditions than those required for pyrolysis. AcknowledgmentWe acknowledge the financial support of the Exxon Teaching Fellowship Program. We thank Drs. John Obst and Roger C. Pettersen of the USDA Forest Products Laboratory, Madison, WI, for providing GC/MS analyses. Registry No. Ligninphenyl ether, 101-84-8. Literature Cited Bredenberg. J. B-son; Ceylan, R. fuel 1983, 62. 342. Bredenberg. J. &son; Huuska, M.; Raty, J.; Korpio, M. J . Cstal. 1982, 77, 242. Connors, W. J.; Johanson, L. N.; Sarkanen, K. V.; Winsiow, P. Holzforschung 1980, 3 4 , 29. Domburg, 0. E.; Sergeeva, V. N.; Kalninsh, A. I. Therm. Anal., Proc. Int. Conf. 3rdThe liquefaction of different coals slurried in Koppers' creosote oil at short contact time (12 min) was studied at different reaction temperatures (300-450 "C). The influence of tetralln and hydrogen on short contact time (SCT) liquefaction ylelds and vehicle Incorporation was monitored. The data support the following concepts: (1) The conversion to tetrahydrofuran (THF) and pentane solubles of the reaction products increased with increasing temperature in all cases.(2) The presence of tetraiin or hydrogen enhanced the conversion to THF and pentane solubles; when both tetralln and hydrogen were present, the effects were additive for conversion to pentane solubles but not additive for conversion to THF solubles. (3) Both high temperature and the presence of a hydrogen source minimized vehicle incorporation into the coal and coal products.

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