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应用红外光谱在线监测2,3,4-戊三酮-3-肟和水合肼合成4-氨基-3,5-二甲基吡唑的反应过程,采用多元曲线分辨-交替最小二乘法(MCR-ALS)以及直观推导式演进特征投影法(HELP)等化学计量学方法对所获得的实时动力学红外光谱数据矩阵进行解析,获得了反应物、中间体及产物的浓度变化曲线和对应的红外光谱。并将两种方法的分析结果进行比较,得出可相互验证的一致结论,以此推出该反应的合理机理。结果表明实验所选的化学计量学方法结合在线红外可以快速、有效反映4-氨基-3,5-二甲基吡唑合成过程中各组分的浓度变化和红外光谱的变化,对其反应机理的研究具有重要的指导意义。
The reaction process of 2,3,4-pentanetrione-3-oxime and hydrazine hydrate in the synthesis of 4-amino-3,5-dimethylpyrazole was monitored by infrared spectroscopy. The multivariate curvilinear resolving-alternating least square method -ALS) as well as the intuitive derivatization evolution projection (HELP) and other stoichiometric methods were used to analyze the real-time kinetic IR spectra data matrix. The concentration curves of reactants, intermediates and products were obtained and the corresponding infrared spectrum. The results of the two methods are compared and the agreement conclusion of mutual verification is obtained, in order to deduce the reasonable mechanism of the reaction. The results show that the selected stoichiometry combined with on-line infrared can quickly and effectively reflect the changes of concentration and infrared spectra of 4-amino-3,5-dimethylpyrazole and the reaction mechanism Research has important guiding significance.