甲基氯硅烷低沸物的分离分析  

Separation and Analysis of Low-boiling Residues of Methylchlorosilanes

作　　者：周婷婷[1] 陈关喜[1,2] 吴清洲[1,2] 冯建跃[2] 

机构地区：[1]浙江大学化学系,浙江杭州310027 [2]浙江大学分析测试中心,浙江杭州310027

出　　处：《分析测试学报》2009年第12期1448-1451,共4页Journal of Instrumental Analysis

基　　金：浙江省科技计划资助项目(2007F70058);浙江省重大科技专项(优先主题)工业资助项目(2008C11114)

摘　　要：选用DB-624毛细管色谱柱,用气相色谱法对直接法合成的26种甲基氯硅烷低沸物(LBR)组分(其中包括难分离的物质对甲基二氯硅烷和2-甲基-2-丁烯)进行分离。考察了柱温和载气流速对分离效果的影响,发现柱温和载气流速均较低时,分离效果较好。采用气相色谱质谱联用和气相色谱保留时间对照2种方法对组分进行了定性分析,根据色谱保留时间和质谱图的信息,确定了LBR组分结构,并对其进行了定量分析。结果表明,四甲基硅烷、二甲基氯硅烷和甲基二氯硅烷是LBR的主要活性成分,而2-甲基-1丙-烯、2-甲基丁烷和2甲-基-2丁-烯是LBR的主要杂质。方法操作简便、快速、效率高,适用于甲基氯硅烷生产控制中的快速分析和其工业分离的方法研究。26 components of low-boiling residues of methylchlorosilanes（LBR） from direct synthesis process, including the most important difficult-to-separate pair of methyldichlorosilane and 2-methyl- 2-butene, were well separated on a DB-624 capillary column. Effect of column temperature and carrier gas flow rate on resolution of LBR was investigated. The result indicated that lower column temperature and carrier gas flow rate were more favorable to the separation. Under the optimal conditions, 26 LBR components were qualitatively analyzed by gas chromatography -mass spectrometry （GC -MS） and gas chromatography（GC） on the basis of retention time and molecular structure of LBR constituents. Then they were quantitatively analyzed by GC with the flame ionization detector （FID） by peak area normalization method. The results showed that tetramethylsilane, dimethylchlo- rosilane and methyldichlorosilane were the dorminant active ingredients of LBR, and 2-methyl-l-propene, 2-methylbutane and 2-methyl-2-butene were the major impuritys. The method was simple, fast, and efficient, and was suitable for the rapid analysis and separation of production control for the methylchlorosilanes.

关 键 词：甲基氯硅烷 低沸物 毛细管色谱柱 气相色谱 气相色谱质谱联用 

分 类 号：O657.71[理学—分析化学]