High-temperature coal tar was extracted with petroleum ether (PE) under ultrasonic irradiation and the extracts were analyzed with gas chromatograph/mass spectrometer. The acearylene fractions including acenaphthyle...High-temperature coal tar was extracted with petroleum ether (PE) under ultrasonic irradiation and the extracts were analyzed with gas chromatograph/mass spectrometer. The acearylene fractions including acenaphthylene, aceanthrylene and cyclopentapyrene were enriched together and named E, which was then transferred to a car- tridge in Isolera-One flash chromatography. Three groups of compounds were eluted out with ethyl acetate/PE mixed solvent (volume ratio 1:9) and named E1, E2 and E3 according to their main components. Acenaphthylene accounted for 78.2% in El, aceanthrylene 71.6% in E2 and cyclopentapyrene 75.9% in E3, respectively. The three groups of acearylenes were purified by Sephadex LH-20 column chromatography with ethanol/cyclohexane mixed solvent (vol- ume ratio 1:4), and then confirmed with nuclear magnetic resonance spectrometer. This method indicates that flash chromatography has a good effect on separating the compounds with a similar structnre after extraction under ultrasonic irradiation.展开更多
基金Supported by National Natural Science Foundation of China for Innovative Research Group(No.50921002)the Program of the Universities in Jiangsu Province for Development of High-Tech Industries(No.JHB05-33)the Fundamental Research Funds for the Central Universities (China University of Mining and Technology,No.2010ZDP02B03)
文摘High-temperature coal tar was extracted with petroleum ether (PE) under ultrasonic irradiation and the extracts were analyzed with gas chromatograph/mass spectrometer. The acearylene fractions including acenaphthylene, aceanthrylene and cyclopentapyrene were enriched together and named E, which was then transferred to a car- tridge in Isolera-One flash chromatography. Three groups of compounds were eluted out with ethyl acetate/PE mixed solvent (volume ratio 1:9) and named E1, E2 and E3 according to their main components. Acenaphthylene accounted for 78.2% in El, aceanthrylene 71.6% in E2 and cyclopentapyrene 75.9% in E3, respectively. The three groups of acearylenes were purified by Sephadex LH-20 column chromatography with ethanol/cyclohexane mixed solvent (vol- ume ratio 1:4), and then confirmed with nuclear magnetic resonance spectrometer. This method indicates that flash chromatography has a good effect on separating the compounds with a similar structnre after extraction under ultrasonic irradiation.