Catalytic hydroprocessing of SRC-II heavy distillate fractions. 1. Preparation of the fractions by liquid chromatography

Abstract

= standard normal variable, dimensionless Greek Symbols a = fraction J ? ( ) = gamma function p,(t) = mean of H(c,t), g p,(t) = mean of G(n,t), dimensionless pT = mean cycle time, min puw = mean of F(w), g uJt) = standard deviation of H(c,t), g u, = standard deviation of G(n,t), dimensionless UT = standard deviation of the cycle time, s u, = standard deviation of F(w), g Liquid chromatography, with columns containing cation-exchange resin and clay-supported Fe2Ci6, was used on a preparative scale to separate 10 10-batches of a coacclertved liqukl (SRCII heavy distkte) Into nine fractions, each consisting of chemically similar compounds. The fractions are strong, weak, and very weak bases: strong, weak, and very weak acids; neutral oils; neutral resins; and asphattenes. Each fraction has been characterized spectroscopically, and representative structures have been identified. The yleld data indicate good reproducibility in the separations, and the fractions of Bach type have been combined, giving sufficient quantities to allow high-pressure microreactor experiments characterizing the catalytic hydroprocessing of each fraction individually.One kilogram of SRCII heavy dlstl#ete has been separated into nine fractkns by pmparative liquid chromatography.The fractions (strong, weak, and very weak bases; strong, weak, and very weak acids; neutral resins; and asphaltenes) have been characterized in detail by elemental analysis, 'H NMR at 80 and 600 MHz, 13C NMR, IR, mass spectrometry, vapor phase osmometry, and other techniques. The results have been used as a basis for postulating representative molecular structures of each fraction. The fractions are to be used individually in high-pressure microreactor studies of catalytic hydroprocessing.

Catalytic hydroprocessing of SRC-II heavy distillate fractions. 6. Hydroprocessing of the bases and neutral resins

“…The large peak at 50.76 min in the former is indicative of pyrene, added as an external standard. The fact that almost as many peaks were detected with the nitrogen-specific Hall detector as with the unspecific flame ionization detector shows that most of the compounds in the fraction contain nitrogen, as expected from the separation chemistry (Petrakis et al, 1983a(Petrakis et al, , 1983b.…”

“…Therefore, the identifications stated in the next few paragraphs should be considered only tentative. From its weakly basic nature, the fraction was expected to contain aminophenols (Petrakis et al, 1983a(Petrakis et al, , 1983b. But aminophenol and its methyl derivatives were not observed.…”

“…Here, we consider the basic and neutral resins fractions, which contain most of the organonitrogen components of the coal liquid. The details of the preparation and characterization of the fractions have been reported in the first papers of this series (Petrakis et al, 1983a(Petrakis et al, , 1983b.The strong, weak, and very weak base fractions account for about 10% of the total heavy distillate. In a typical compound, nitrogen is present in -NH2 groups or in sixmembered rings.…”

“…Further details of these fractions are available elsewhere (Petrakis et al, 1983a(Petrakis et al, , 1983bKatti, 1984). Individual compounds identified in the fractions are mentioned below.…”

Optimization of reaction variables and macrokinetics for the hydrodeoxygenation of full range low temperature coal tar

“…Furimsky [30] studied the HDO of industrial feeds, such as gas oils derived from thermal hydrocracking of heavy oils using a Co-Mo/c-Al 2 O 3 catalyst. Various investigations on the hydrogenation kinetics of phenolic compounds of coal-derived liquids [16,[31][32][33][34]. Chon and Allen [35] conducted studies using a batch reactor system on the HDO kinetics of phenols over a sulfided Ni-Mo/Al 2 O 3 catalyst.…”