在线红外与量热技术联用分析噻吩酯合成反应过程

Analysis on Thiophene Ester Synthesis Process by Combination of Online Infrared and Calorimetry

为了清晰认知和评估化学反应过程,明确反应优化的方向,建立了基于反应量热仪和在线红外联用的方法,用于原位检测釜式反应系统。该方法利用反应量热仪对釜内样品温度等变量进行测量及精准控制,并结合在线红外光谱仪对物质官能团变化进行的连续实时检测,可同时获取化学反应过程实时放热热流、热转化率等热力学信息以及样品中反应物、产物比例随时间变化的趋势。通过测定比较不同工艺条件下的反应结果,考察工艺条件对反应进程、最终产物的影响。将该联用方法应用于噻吩酯合成工艺的结果表明,调整工艺温度可改善最终产物质量,同时反应热危险性可控。这种基于在线红外与量热技术联用的原位反应过程研究方法,可应用于化学反应过程的研究并有效实现对反应过程的认知。

In order to clearly understand,evaluate the chemical reaction process,and determine the direction of reaction optimization,an in-situ detection system was developed to monitor the reaction in a batch reactor.In this method,the reaction calorimeter was used to accurately control and measured the process variables such as temperature,and the online infrared(IR)was used for continuous real-time detection of changes in the functional groups of the substance.The real-time exothermic heat flow,heat conversion and other thermodynamic information of the chemical reaction process,and the trend of the proportion of reactants and products in the sample over time could be obtained by this combination.By measuring and comparing of reaction data under different process conditions,the effects of process conditions on the reaction process and the final product are investigated.The method was applied to the thiophene ester synthesis process,and it was proved that adjusting the process temperature could improve the quality of the final product,and the thermal danger of the reaction could be controlled.The in-situ measurement and analysis method based on the combination of online IR and calorimetric technology could be applied to research and cognitive chemical reaction processes.