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Dense-gas fractionation of mixtures of petroleum macromolecules

机译：石油大分子混合物的浓密气体分馏

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Dense-gas extraction (DGE) was used to fractionate a petroleum pitch feedstock of broad molecular weight distribution (MWD) into selected oligomeric constituents. The DGE process was carried out in a semibatch mode using the solvent toluene (T-c = 318.6 degrees C, P-c = 41.1 bar) and a pitch charge of 10-15 g. A packed column with reflux produced the equivalent of several equilibrium stages. The apparatus was operated at near and supercritical temperatures, with the stillpot at 320 degrees C and the column temperature increasing linearly up to the reflux condenser temperature of 360 degrees C. Operating pressures were determined by the conditions required to extract a given oligomer and varied from 44 to 84 bar. Using a monomer-rich petroleum pitch feed (MW,, = 299, PDI = 1.10), a dimer-rich extract with a purity approaching 90% (MW, = 521, PDI = 1.07) was obtained, with the remaining residue (MW,, = 883, PDI = 1.24) consisting of 95% trimer and higher oligomers. MALDI-TOF mass spectrometry was used to determine the MWD of the feed pitch and pitch fractions, with a unique matrix being used to enhance the response of higher MW species. The combination of DGE for separation and MALDI for accurate MW information is a powerful new technique for the molecular characterization of insoluble, high MW fossil fuels. (c) 2004 Elsevier B.V. All rights reserved.
机译：稠气萃取（DGE）用于将宽分子量分布（MWD）的石油沥青原料分馏为选定的低聚组分。 DGE工艺使用溶剂甲苯（T-c = 318.6摄氏度，P-c = 41.1巴）和沥青装料量为10-15 g，以半间歇模式进行。带有回流的填充柱产生了几个平衡阶段的当量。该设备在近临界温度和超临界温度下操作，釜在320摄氏度，柱温线性增加，直到回流冷凝器温度达到360摄氏度。操作压力由提取给定低聚物所需的条件决定， 44至84巴。使用富含单体的石油沥青进料（MW，= 299，PDI = 1.10），获得纯度接近90％（MW，= 521，PDI = 1.07）的富含二聚体的萃取物，剩余的残余物（MW ，＝ 883，PDI ＝ 1.24）由95％的三聚体和更高的低聚物组成。 MALDI-TOF质谱用于确定进料沥青和沥青馏分的MWD，并使用独特的基质来增强较高MW物质的响应。 DGE用于分离和MALDI用于精确兆瓦信息的结合是一种用于对不溶性高兆瓦矿物燃料进行分子表征的强大新技术。 （c）2004 Elsevier B.V.保留所有权利。

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