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首页> 外文会议>International Symposium on Supercritical Fluids Tome 1: Natural Products, Process amp; Equipment Development; 20030428-20030430; Versailles; FR >MIXTURES OF PETROLEUM MACROMOLECULES: THEIR FRACTIONATION, CHARACTERIZATION, AND PHASE BEHAVIOR
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MIXTURES OF PETROLEUM MACROMOLECULES: THEIR FRACTIONATION, CHARACTERIZATION, AND PHASE BEHAVIOR

机译：石油大分子混合物：其分馏，表征和相行为

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摘要

Dense-gas extraction is being investigated for the fractionation of petroleum macromolecules, with an emphasis on those carbonaceous pitches that can serve as precursors for advanced carbon materials. For this investigation, we synthesized a model pitch from pure anthracene so that a relatively well-defined material would be available for study. A dense-gas extraction apparatus was designed and constructed for semi-continuous operation at temperatures and pressures to 400℃ and 200 bar, respectively. The unit was designed for the fractionation of 3-10 g of pitch per run and can be operated isothermally; with a linear, positive temperature gradient; or with a linear, negative temperature gradient across the length of the column. If properly applied, such a gradient can be expected to generate a liquid reflux stream and thus improve the purity of the overhead cuts that are obtained. Experiments were carried out using either supercritical pentane or toluene as the extractive solvents, with temperature gradients (ΔT's) of-20, 0, and +20℃ being evaluated. MALDI-TOF-MS was used to determine the molecular weight distribution of selected overhead cuts, and of the residue remaining in the stillpot. Results to date indicate that the technique has potential for the separation of pitches into their constituent oligomers. A pure monomer cut was obtained with pentane and a ΔT of -20℃, while a pure dimer cut was isolated by using toluene as the extractive solvent.
机译：目前正在研究稠密气体萃取技术用于石油大分子的分离，重点是可以用作高级碳材料前体的碳质沥青。对于此研究，我们从纯蒽合成了模型沥青，因此可以使用定义相对明确的材料进行研究。设计并构造了一种高密度气体萃取设备，可在温度和压力分别达到400℃和200 bar的条件下进行半连续操作。该装置设计为每次运行可分馏3-10 g的沥青，并且可以等温运行；具有线性正温度梯度；或在整个色谱柱长度上具有线性的负温度梯度。如果适当地施加，可以预期这种梯度会产生液体回流，从而提高所获得的塔顶馏出物的纯度。使用超临界戊烷或甲苯作为萃取溶剂进行实验，评估温度梯度（ΔT's）为-20、0和+ 20℃。 MALDI-TOF-MS用于确定所选塔顶馏分和蒸馏釜中残留残留物的分子量分布。迄今为止的结果表明，该技术具有将沥青分离为其组成低聚物的潜力。用戊烷和-20℃的ΔT可获得纯单体馏分，而用甲苯作为萃取溶剂则分离出纯二聚体馏分。

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