Establishmant Of Analysis Method In Catalytic Oxidation Of Mesitylene To Trimesic Acid By Air

During the reaction of catalytic oxidation of mesitylene by air in the gas-liquid phase to synthesize trimesic acid as well as the correlative process, with the aim of controlling the product's quality and improving its reaction yield, it's necessary to bulid a set of reliable and integral analysis methods. In the research, the reaction components analysis methods, such as chromatographic analysis, mass spectral analysis, ultra-red absorption spectroscopy, atomic absorption spectrophotometer, chemical titrimetric analysis are tried. This paper puts the emphasis on these analysis means and sets up correlative analysis method.As to the gasometric analysis, double column parallel connection is used to separate O₂,N₂,CO₂ under ambient temperature and vapour-phase chromatography TCD is used to have a quantitative analysis. For the liquid, the DMF is adopted as internal standardand and with fixed phase of OV-101 of 15 meters capillary column, vapour-phase chromatography FID is successfully used to have a quantitative analysis on mesitylene and acetic acid. As to the high polarity, high boiling point resultant—trimesic acid, the analysis methods of infrared spetrum, gas chromatography-mass spectroscopy, vapour-phase chromatography, acid number titration and so on are seperately used to characterize its property. Infrared spetrum and gas chromatography-mass spectroscopy are used to have a qualitative analysis on the resultant and are compared with the stand diagram. Sulfuric acid-methanol esterification and rapid esterification are used to prepare the trimesic acid trimethyl-ester and have a FID quantitative analysis. So that we make sure the purity of trimesic acid in the resultant and also we have an acid alkali titration on the resultant to get its acid number, in order to verify the purity of trimesic acid in the resultant.The above analysis methods are easily to operate and apply. They provide a great deal of data for chemical process controlling and optimizing, and are successfully applied with catalytic oxidation of mesitylene by air in the gas-liquid phase to synthesize trimesic acid and the correlative chemical process.