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提出用衍生物-NMR表征石油中的有机硫结构的方法。在四氟硼酸银的存在下,分别用2H或13C同位素富集的碘甲烷,把石油中的有机硫定量地转变为相应的甲基锍盐,然后用2HNMR和13CNMR表征硫化物的结构。给出了一些模型甲基锍盐的2HNMR和13CNMR化学位移值。分析结果表明,石油中噻吩类为苯并噻吩型等结构;硫醚为脂肪硫醚、二苯硫醚及α-萘基甲基硫醚等;阿拉伯原油样品中,大约70%的硫化物为噻吩类化合物,其余为硫醚类化合物;有机硫化物的甲基化转化率为65%~87%。
A new method to characterize the organosulfur structure in petroleum using derivative-NMR is proposed. The organosulfur in oil was quantitatively converted to the corresponding methylsulfonium salt in the presence of silver tetrafluoroborate by methyl iodide enriched with 2H or 13C, respectively, and the structure of the sulfide was characterized by 2HNMR and 13CNMR. The 2HNMR and 13CNMR chemical shifts of some methylsulfonium salts are given. The analytical results show that the thiophenes in petroleum are of the benzothiophene type and the like; the thioethers are aliphatic thioethers, diphenylsulfides and α-naphthyl methylsulfides, etc. In the samples of Arab crude oil, about 70% of the sulfides are Thiophene compounds, the rest is thioether compounds; the methylation conversion rate of organic sulfides is 65% ~ 87%.