| Acetylferrocene is an important organic synthetic intermediate,and there are currently various synthesis methods available,with relatively mature synthesis processes.However,conventional detection methods such as infrared spectroscopy,ultraviolet spectroscopy,spectrophotometry,and high-performance liquid chromatography have long detection times,complex operations,and cannot quickly analyze the content of acetylferrocene in synthesized samples.Moreover,these methods are offline detection and cannot monitor the content of acetylferrocene in real-time during the ferrocene acetylation process.This study aims to investigate the rapid analysis of the content of each component in the ferrocene acetylation sample,real-time online monitoring of each component during the ferrocene acetylation process,and the reaction kinetics.(1)A rapid analysis model for the content of ferrocene,acetylferrocene,and 1,1’-diacetylferrocene in ferrocene acetylation samples was established using infrared spectroscopy combined with vector angle conversion method.Orthogonal experiments were designed based on literature to synthesize ferrocene acetylation samples as analytical samples.The infrared spectra were collected and analyzed by liquid chromatography.The vector angle conversion method was used to calculate the angle value θ between the series of sample spectra and the reference spectrum,and the linear fitting between the angle value θ and the true liquid content was performed to obtain the analysis model for the rapid analysis of ferrocene,acetylferrocene,and 1,1’-diacetylferrocene in samples.The correlation coefficients of the established model were 0.9977,0.9962,and 0.9934,respectively,and the relative errors were-5.97% to 9.90%,-4.94% to 6.51%,and-1.44%to 10.48%.The RSD values of the method were 0.39% to 1.89%,0.30% to 0.75%,and1.23% to 3.04%.The results showed that the established method can be used for the rapid analysis of the content of each component in ferrocene acetylation samples.(2)A rapid online analysis model was established for monitoring the content of ferrocene,acetylferrocene,and 1,1’-diacetylferrocene during the acetylation of ferrocene using infrared spectroscopy combined with angle transformation method.During the acetylation process,process samples were collected and their infrared spectra were analyzed.The angle value θ between the series of process spectra and the reference spectrum was calculated using the vector angle transformation method.A model for analyzing the concentration of ferrocene,acetylferrocene,and 1,1’-diacetylferrocene in the process samples was established based on the relationship between the angle value θ and the liquid phase concentration.The model showed good correlation coefficients(r=0.9934,0.9941,0.9715)and relative errors ranging from-9.36% to 4.87%,-12.06% to 4.04%,and-16.55% to 8.62%.The established method is convenient and fast for the real-time monitoring of multiple components in the acetylation process of ferrocene.(3)Under different reaction conditions,infrared spectra were collected during the acetylation of ferrocene,and the angle value θ between the spectra of the reaction and the reference spectra was calculated using the vector angle transformation method.The obtained angle values θ were then used as inputs for an established online fast analysis model of acetyl ferrocene,which provided the concentrations of acetyl ferrocene at various time intervals.Two sets of experiments were selected,and the reaction order of ferrocene monoacetylation was determined to be first-order using the method of least squares.The correlation coefficients of the established models were 0.9697 and 0.9721.The results show that the angle value θ obtained by transforming the infrared spectra can be used to determine the reaction order and calculate the rate constant,providing a new approach for kinetic studies of reactions. |
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