化学计量学和红外光谱研究3,5-二氨基-1,2,4-三唑合成机理  

Study on Synthetic Reaction Mechanism of 3,5-Diamino-1,2,4-triazole by Chemometrics and Infrared Spectroscopy

作　　者：蔡玲玲[1] 王伯周[2] 焦龙[3] 葛忠学[2] 覃光明[2] 李华[1] 

机构地区：[1]西北大学化学与材料科学学院,西安710069 [2]西安近代化学研究所,西安710065 [3]西安石油大学化学化工学院,西安710065

出　　处：《分析化学》2011年第6期920-924,共5页Chinese Journal of Analytical Chemistry

基　　金：973计划(No.61374xx);国家自然科学基金(No.20975081)资助项目

摘　　要：通过红外光谱在线监测3,5-二氨基-1,2,4-三唑(DAT)的合成过程,应用多元曲线分辨-交替最小二乘法(MCR-ALS)对过程中获得的光谱数据矩阵进行解析,推导出合理的反应机理。反应以水为背景,依次加入二氰二胺与二盐酸肼固体,用红外探头监测反应全过程。用MCR-ALS法对所得光谱数据进行解析,得到反应物、中间体和产物的浓度变化及纯物质的光谱曲线。所得结论与文献吻合很好,表明MCR-ALS方法结合在线红外光谱是研究反应机理的有效手段,且对反应路线的选择有指导意义。Online Infrared spectrum was used for monitoring the reaction process of synthesizing 3,5-diamino-1,2,4-triazole（DAT）.The obtained data matrix of IR was analyzed by multivariate curve resolution-alternating least squares method（MCR-ALS） and reasonable mechanism was deduced.The water was used as the background for reaction,then cyanoguanidine and hydrazine dihydrochloride were added in turn,which was detected by IR probe.The concentration profiles and spectra of reactants,intermediates and product were determined by analyzing the spectral data using MCR-ALS method.The obtained results were coincided with literature,which showed that the reaction mechanism could be deduced well by MCR-ALS method combined with online infrared spectrum.It could also provide significant guidance to the choice of reaction.

关 键 词：红外光谱 渐进因子分析 多元曲线分辨-交替最小二乘法 三唑衍生物 反应机理 

分 类 号：O621.3[理学—有机化学]