抚顺乙烯焦油的精馏分离与气相色谱-质谱联用分析

摘要

为避免乙烯焦油作为燃料粗放燃烧造成的芳烃资源浪费与环境污染,我们以抚顺乙烯焦油为原料,常压蒸馏切割<280℃馏分,然后采用填充柱进行常压精馏,将<280℃馏分切割为12个馏分段(40~150℃、150~170℃、170~180℃、180~190℃、190~200℃、200~210℃、210~220℃、220~230℃、230~240℃、240~250℃、250~260℃和260~280℃),以达到对抚顺乙烯焦油的精馏分离.以HP-5MS毛细管填充柱为色谱柱,对得到的12个馏分段进行气相色谱-质谱联用定性、定量分析,为乙烯焦油中芳烃的提取和乙烯焦油深加工利用提供具有指导价值的分析数据.结果显示,抚顺乙烯焦油<280℃馏分占焦油总量的52.2%,主要由1~4芳香烃组成.单环、三环和四环芳烃质量分数较少,单环芳烃主要为苯的衍生物,质量分数为5.8%,3环和4环芳烃占2.998%,主要为苊、芴、蒽、菲、芘等.抚顺乙烯焦油中质量分数最多的双环芳烃为萘,其次为β-甲基萘、α-甲基萘和1,4-二氢萘,它们在各馏分段的最高分布分别为41.152%、16.729%、12.089%和9.046%.由此乙烯焦油可作为提取高附加值芳环类精细化工产品的良好原料.%In order to avoid the aromatics waste and environmental pollution caused by ethylene bottom oil as a crude fuel for combustion, Fushun ethylene bottom oil was subjected to atmospheric distillation to obtain a fraction below 280 ℃.To achieve separation of ethylene bottom oil, the fraction below 280 ℃ was cut into 12 fractions(40~150 ℃, 150~170 ℃, 170~180 ℃, 180~190 ℃.190~200 ℃, 200~210 ℃.210~220 ℃, 220~230℃, 230~240℃, 240~250℃, 250~260℃.260~280℃) by atmospheric distillation unit equipped with packed columns.The obtained 12 fractions were analyzed qualitatively and quantitatively by gas chromatography/mass spectrometry with an HP-5MS capillary column as the stationary phase.We hope it could provide valuable analytical data for the extraction of aromatic hydrocarbons, and the deep processing and utilization of ethylene bottom oil.The results indicate that the distillate below 280℃account for 52.2%of the total amount of ethylene bottom oil in Fushun, and mainly contained aromatic hydrocarbons with 1 to 4 rings.The mass fraction of monocyclic, tricyclic and tetracyclic aromatic hydrocarbons is small. The monocyclic aromatic hydrocarbons are mainly derivatives of benzene and indene that account for 5.8% and 6.172%of ethylene bottom oil in Fushun, respectively.The tricyclic and tetracyclic aromatic hydrocarbons account for 2.998%and mainly are acenaphthene, fluorene, anthracene, phenanthrene, pyrene and so on. The most abundant bicyclic aromatic hydrocarbons in Fushun ethylene bottom oil are naphthalene, followed byβ-methylnaphthalene, α-methylnaphthalene and 1, 4-dihydronaphthalene with mass fraction of 41.152%, 16.729%, 12.089%and 9.046%, respectively.This research shows that ethylene bottom oil in Fushun can be used as good feedstock for extracting high value-added aromatic fine chemicals.