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本文报道在加温加压反应条件下原位红外光谱的测试方法,包括了加温加压红外光谱样品槽的研制;连续循环式和釜式加温加压络合催化反应-原位红外光谱联用装置的建立,以及应用该装置检测不稳定催化活性中间络合物的方法。实验表明,本方法既可以定性和定量地测出用一般红外光谱方法所不能发现的活性催化络合物的特征吸收峰,又可追踪各活性中间物的消长和确定各基元反应的次序,同时还可用于研究基元反应动力学和鉴定对空气敏感的络合物的结构,是研究均相反应机理的工具。
In this paper, the method of in-situ IR spectroscopy under heating and pressure reaction conditions is reported, including the development of a sample cell under heating and pressure infrared spectroscopy; the continuous cyclic and autoclave pressurized catalytic reaction - in situ FTIR The establishment of the combined device and the method for detecting the unstable catalytically active intermediate complex by using the device. Experiments show that the method can not only qualitatively and quantitatively detect the characteristic absorption peak of the active catalytic complex which can not be found by the general infrared spectroscopy method but also trace the growth of each active intermediate and determine the sequence of each elementary reaction, At the same time, it can be used to study elementary reaction kinetics and to identify the structures of air-sensitive complexes. It is a tool to study the homogeneous reaction mechanism.