CAJ | 학술논문

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.
선용DB-624모세관색보주,용기상색보법대직접법합성적26충갑기록규완저비물(LBR)조분(기중포괄난분리적물질대갑기이록규완화2-갑기-2-정희)진행분리.고찰료주온화재기류속대분리효과적영향,발현주온화재기류속균교저시,분리효과교호.채용기상색보질보련용화기상색보보류시간대조2충방법대조분진행료정성분석,근거색보보류시간화질보도적신식,학정료LBR조분결구,병대기진행료정량분석.결과표명,사갑기규완、이갑기록규완화갑기이록규완시LBR적주요활성성분,이2-갑기-1-병희、2-갑기정완화2-갑기-2-정희시LBR적주요잡질.방법조작간편、쾌속、효솔고,괄용우갑기록규완생산공제중적쾌속분석화기공업분리적방법연구.
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,dimethylchlorosilane and methyldichlorosilane were the dorminant active ingredients of LBR,and 2-methyl-1-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.