甲基二乙氧基苯乙基硅烷的合成及气相色谱法测定  

Synthesis and determination of the phenylethylmethyldiethoxysilane by gas chromatography

作　　者：叶志刚[1,2] 史鸿鑫[1] 

机构地区：[1]浙江工业大学绿色化学合成技术国家重点实验室培育基地,杭州310032 [2]九江学院化工学院,九江243002

出　　处：《分析试验室》2015年第5期566-569,共4页Chinese Journal of Analysis Laboratory

摘　　要：建立了苯乙烯与甲基二乙氧基硅烷硅氢化反应体系中各组分含量测定的气相色谱检测方法。在GC-14B气相色谱仪(HP-5毛细管柱、FID检测器)上,以氮气为载气,采用程序升温法对各组分进行定量分析。在本实验色谱条件下,常用作基准物的正庚烷和苯的谱峰重合;而采用N,N-二甲基苯胺作为基准物质,5种组分的谱峰分离效果较好,苯乙烯、甲基二乙氧基硅烷及两种加成产物的相对质量校正因子测定值分别为0.7006,1.998,1.530,1.530;而用有效碳数法计算的理论值分别为0.8431,2.1465,1.2706,1.2706。最后,用经校正的面积归一化法测定了硅氢化反应体系中各组分含量。方法可用于硅氢加成产物的定量分析及质量控制。A method was developed for the content determination of the reactants and products of hydrosilylation between styrene and methyldiethoxysilane. A GC method was adopted. Quantitative analysis was performed on a HP-5 capillary column using nitrogen gas as a cartier gas and FID as a the detector by temperature programming. Under the experimental conditions, the spectral peaks of methyldiethoxysilane, n-heptane and benzene were overlapped; but separation effecl of five components is good with N, N-dimethylaniline as the standard substance of the reaction system. The correction factors of styrene, methyldiethoxysilane, a-phenylethylmethyldiethoxy silane and 13-phenylethymethyldiethoxy silane were determined, and their measured values were 0. 7006,1. 998, 1. 530 and 1. 530, respectively. Theoretical values of four components obtained from the effective carbon number law were 0. 8431, 2. 1465, 1. 2706 and 1. 2706, respectively. The content of each component was measured by the area correction normalization method. The method is simple, accurate, sensitive and reproducible, which can be used in the quantitative analysis and quality control of the hydrosilylation product.

关 键 词：硅氢加成 气相色谱 校正因子 面积归一化法 有效碳数 

分 类 号：O657.7[理学—分析化学]