The FT-i.r. and 1H n.m.r. spectroscopic analyses of oils or maltenes from a Spanish lignite (Utri... more The FT-i.r. and 1H n.m.r. spectroscopic analyses of oils or maltenes from a Spanish lignite (Utrillas, Teruel), are reported. These oils were obtained by depolymerization with alkyl aromatic ethers (anisole, 3-methylanisoleand 1,3-dimethoxybenzene) catalyzed by Lewis acids ZnCl2, AlCl3, SbCl3and BF3 (as boron trifluoride etherate), at atmospheric pressure and temperatures <220 °C. Bands due to aromatic ethers in the i.r. and n.m.r. spectra of the oils obtained by depolymerization indicate solvent incorporation. Oils obtained by direct lignite extraction showed 25% aromatic H and some Hα (≈3%) without OH groups. These appeared in some oils obtained by depolymerization with AlCl3 and were due to secondary reactions with the aromatic extract. Oils derived from processes with good yields showed increases in aromaticity. The extent of substitution of aromatic rings in oils obtained by depolymerization was less than for oils directly extracted. All the oils studied show a low degree of condensation.
Summary Two alternative methods, based on Thin-Layer Chromatography (TLC) with Fluorescence Scan... more Summary Two alternative methods, based on Thin-Layer Chromatography (TLC) with Fluorescence Scanning Densitometry have been developed for characterization of heavy liquids from copyrolysis of different kinds of biomass and plastics in autoclaves under inert atmosphere. A conventional TLC system, which includes a vertical developing tank, and a High Performance TLC (HPTLC) system, with a horizontal developing chamber and the use of
1991 International Conference on Coal Science Proceedings, 1991
Publisher Summary This chapter describes the effect of inherent mineral matter and additives on h... more Publisher Summary This chapter describes the effect of inherent mineral matter and additives on hydrogenation of Spanish coals. The effect of mineral matter present in coal has been widely studied in hydrogenation processes. The chapter presents the results of the hydrogenation experiments runs carried out with original and demineralized coals, with and without additives. The conversions obtained with hydrogenations of the demineralized coals decrease drastically in comparison with the original coals, which reveals that the inherent mineral matter plays an important role in coal hydrogenation. This could suggest that the demineralization provides a higher interaction between reactive groups, and, in this way, the hydrocarbonated frame of coal would be more difficult to make soluble; moreover, the removal of mineral matter would facilitate the condensation of the carbonaceous fragments from thermolysis. The hydrogenation reactions performed on the original coals without and with additives gave conversions and liquid productions which can be considered as high and very high, respectively. The additives proved to be moderately active and gave a moderate increase in conversion and liquid production in most experiments.
1991 International Conference on Coal Science Proceedings, 1991
Publisher Summary This chapter discusses upgrading of liquids from direct coal liquefaction. In a... more Publisher Summary This chapter discusses upgrading of liquids from direct coal liquefaction. In a study described in the chapter, liquids obtained by direct coal liquefaction were deasphalted to reduce the heteroatom content and the catalyst deactivation in hydrotreating. Two methods were tried: (1) the deasphalting with hexane in autoclave at 100°C of temperature and 20 kg/cm2 pressure and (2) ultrasonic disgregation in hexane. The latter method was chosen because of the higher yields obtained. The extracted oils were hydrogenated in a continuous hydroprocessing unit. Two different catalysts were used: (1) Harshaw HT-400E containing 3 wt% CoO and 15 wt% MoO3 on gamma alumina, and (2) Harshaw HT-500E containing 15 wt% MoO3 and 3.5 wt% NiO on gamma alumina. They were sulfided for 4 h at 400°C of temperature and atmospheric pressure in the presence of a flowing stream of hydrogen containing 10% H2S.
JPC – Journal of Planar Chromatography – Modern TLC
Classic saturates, aromatics, resins, and asphaltenes (SARA) analysis has long enabled the chroma... more Classic saturates, aromatics, resins, and asphaltenes (SARA) analysis has long enabled the chromatographic separation of complex hydrocarbon-containing products into these four families. This simplification often does not provide sufficient or correct information on the relationship between the composition of the products and the process variables studied. The obtention of profiles by gradient automated multiple development (AMD) is an interesting alternative to obtain extended SARA separations with increasing level of complexity for heavy petroleum products that adequately represent the entirety of the sample. An optimized 20-step gradient based on tetrahydrofuran (THF)‒dichloromethane‒n-heptane over a total migration distance of 83 mm is proposed here to characterize all types of heavy oil products. The combination of ultraviolet (UV)–densitometry (at 201, 228, and 273 nm), fluorescence detection by intensity changes using berberine cation, together with on-plate recording of UV s...
The FT-i.r. and 1H n.m.r. spectroscopic analyses of oils or maltenes from a Spanish lignite (Utri... more The FT-i.r. and 1H n.m.r. spectroscopic analyses of oils or maltenes from a Spanish lignite (Utrillas, Teruel), are reported. These oils were obtained by depolymerization with alkyl aromatic ethers (anisole, 3-methylanisoleand 1,3-dimethoxybenzene) catalyzed by Lewis acids ZnCl2, AlCl3, SbCl3and BF3 (as boron trifluoride etherate), at atmospheric pressure and temperatures <220 °C. Bands due to aromatic ethers in the i.r. and n.m.r. spectra of the oils obtained by depolymerization indicate solvent incorporation. Oils obtained by direct lignite extraction showed 25% aromatic H and some Hα (≈3%) without OH groups. These appeared in some oils obtained by depolymerization with AlCl3 and were due to secondary reactions with the aromatic extract. Oils derived from processes with good yields showed increases in aromaticity. The extent of substitution of aromatic rings in oils obtained by depolymerization was less than for oils directly extracted. All the oils studied show a low degree of condensation.
Summary Two alternative methods, based on Thin-Layer Chromatography (TLC) with Fluorescence Scan... more Summary Two alternative methods, based on Thin-Layer Chromatography (TLC) with Fluorescence Scanning Densitometry have been developed for characterization of heavy liquids from copyrolysis of different kinds of biomass and plastics in autoclaves under inert atmosphere. A conventional TLC system, which includes a vertical developing tank, and a High Performance TLC (HPTLC) system, with a horizontal developing chamber and the use of
1991 International Conference on Coal Science Proceedings, 1991
Publisher Summary This chapter describes the effect of inherent mineral matter and additives on h... more Publisher Summary This chapter describes the effect of inherent mineral matter and additives on hydrogenation of Spanish coals. The effect of mineral matter present in coal has been widely studied in hydrogenation processes. The chapter presents the results of the hydrogenation experiments runs carried out with original and demineralized coals, with and without additives. The conversions obtained with hydrogenations of the demineralized coals decrease drastically in comparison with the original coals, which reveals that the inherent mineral matter plays an important role in coal hydrogenation. This could suggest that the demineralization provides a higher interaction between reactive groups, and, in this way, the hydrocarbonated frame of coal would be more difficult to make soluble; moreover, the removal of mineral matter would facilitate the condensation of the carbonaceous fragments from thermolysis. The hydrogenation reactions performed on the original coals without and with additives gave conversions and liquid productions which can be considered as high and very high, respectively. The additives proved to be moderately active and gave a moderate increase in conversion and liquid production in most experiments.
1991 International Conference on Coal Science Proceedings, 1991
Publisher Summary This chapter discusses upgrading of liquids from direct coal liquefaction. In a... more Publisher Summary This chapter discusses upgrading of liquids from direct coal liquefaction. In a study described in the chapter, liquids obtained by direct coal liquefaction were deasphalted to reduce the heteroatom content and the catalyst deactivation in hydrotreating. Two methods were tried: (1) the deasphalting with hexane in autoclave at 100°C of temperature and 20 kg/cm2 pressure and (2) ultrasonic disgregation in hexane. The latter method was chosen because of the higher yields obtained. The extracted oils were hydrogenated in a continuous hydroprocessing unit. Two different catalysts were used: (1) Harshaw HT-400E containing 3 wt% CoO and 15 wt% MoO3 on gamma alumina, and (2) Harshaw HT-500E containing 15 wt% MoO3 and 3.5 wt% NiO on gamma alumina. They were sulfided for 4 h at 400°C of temperature and atmospheric pressure in the presence of a flowing stream of hydrogen containing 10% H2S.
JPC – Journal of Planar Chromatography – Modern TLC
Classic saturates, aromatics, resins, and asphaltenes (SARA) analysis has long enabled the chroma... more Classic saturates, aromatics, resins, and asphaltenes (SARA) analysis has long enabled the chromatographic separation of complex hydrocarbon-containing products into these four families. This simplification often does not provide sufficient or correct information on the relationship between the composition of the products and the process variables studied. The obtention of profiles by gradient automated multiple development (AMD) is an interesting alternative to obtain extended SARA separations with increasing level of complexity for heavy petroleum products that adequately represent the entirety of the sample. An optimized 20-step gradient based on tetrahydrofuran (THF)‒dichloromethane‒n-heptane over a total migration distance of 83 mm is proposed here to characterize all types of heavy oil products. The combination of ultraviolet (UV)–densitometry (at 201, 228, and 273 nm), fluorescence detection by intensity changes using berberine cation, together with on-plate recording of UV s...
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