煤炭直接液化油中酚类化合物的GC/MS研究  

GC/MS study of phenolic compounds separated from direct coal liquefaction oil

作　　者：毛学锋[1] 高振楠[1] 李文博[1] 胡发亭[1] 史士东[1] 

机构地区：[1]煤炭科学研究总院北京煤化工研究分院,北京100013

出　　处：《煤炭学报》2009年第9期1249-1253,共5页Journal of China Coal Society

基　　金：国家重点基础研究发展计划(973)基金资助项目(2004CB217604);煤炭科学研究总院青年创新基金项目(2006QN35)

摘　　要：使用高效碱液抽提法富集煤液化油中酚类组分，并使用衍生化试剂与该组分定量反应，得到挥发性大幅提高、化合物间分离程度显著改善、适于定性定量分析的酚类硅醚化衍生物．色谱／质谱联用（GC／MS）分析结果表明：酚类组分主要由苯酚、茚酚和萘酚和联苯酚等4类化合物组成，且绝大多数化合物带有烷基侧链．经保留时间指认结合质谱检索，有效鉴定出酚类组分中36种包含1～3环的化合物，并由外标法准确定量出23种化合物的含量．其中苯酚含量为6．24％，甲基苯酚的3个同分异构体含量均超过7．5％．定量结果还显示，烷基苯酚含量最高（57．82％），其次为萘酚（3．29％），再次为茚酚（2．89％）．The trimethylsilyl （TMS） derivatives of phenolic compounds, concentrated from the oil through high efficiency caustic extraction method, were prepared by reacting quantitatively with derivative reagent. The TMS derivatives are suitable for qualitation and quantitation because of their elevated volatility and improved separation degree between one another, the GC/MS result shows that the phenolic compounds are mainly composed of four types of ring structures： phenols, indanols, naphthols and biphenols, and most of them are alkyl substituted. We have identified 36 phenols, which contain 1 -3 rings, using retention time assignation and mass spectrometry matching. Furthermore with the external standard method, the contents of 23 phenols in the oil have been accurately quantitated including the phenol of 6. 24% and all three isomers （o -/m -/p - ） of the cresol of more than 7.5%. The quantitative results also indicate that the alkylphenol is the richest, is 57. 82%, followed by the naphthanol of 3.29% and indanol of 2. 89%.

关 键 词：煤炭直接液化油 酚类化合物 碱液抽提 同分异构体 色谱/质谱联用 

分 类 号：TQ529.1[化学工程—煤化学工程]