航空轮胎专用防焦剂CTP的合成工艺及微观结构表征

Synthesis Process and Microstructure Characterization of Special Coke Inhibitor CTP for Aircraft Tyres

本研究采用连续微化工技术,制得粗品N-环己基硫代邻苯二甲酰亚胺(CTP)防焦剂,脱除部分溶剂,加溶剂油重结晶,得到高品质CTP,含量98.9%,通过FTIR、UV-vis、GC-MS、XRD、1H-NMR对其进行检测和表征,分别从化学键角度、各类π→π^(*)的电子跃迁、GC-MS图谱分析揭示CTP的分子结构。通过CTP的GC-MS图谱分析发现CTP的纯度很高,其杂质主要成分为微量的邻苯二甲酰亚胺,除掉微量的邻苯二甲酰亚胺,是CTP产品品质升级的关键因素。XRD得到了CTP晶胞参数。本文根据1H-NMR谱图和H原子化学位移,推断其氢原子数目和位置,和CTP分子式C14H15O2SN相吻合。本研究为加快CTP新工艺技术工业集成和产业化,提供了基础试验数据和实验依据。

In this study,the continuous microchemical technology was used to prepare crude N-cyclohexylthio-phthalimide(CTP)antibrowning agent.Some solvents were removed.Solvent oil was added for recrystallization to obtain high-quality CTP with a content of 98.9%.The product was detected and characterized by FTIR,UV-vis,GC-MS,XRD and 1H-NMR.The molecular structure of CTP was analyzed by chemical bond,electron transitions ofπ→π^(*)and GC-MS spectra.CTP was showed by GCMS chromatographic analysis.The CTP purity was very high.The impurities were mainly composed of trace phthalimide as raw materials.The removal of trace phthalimide was the key factor to upgrade the quality of CTP products.The CTP cell parameters were obtained by XRD.According to the 1H-NMR spectra and the chemical shift of H atom,it was inferred that the number and location of hydrogen atoms were consistent with the CTP formula C14H15O2SN.This study can provide with basic test data and experimental basis for accelerating industrial technology integration and industrialization of CTP new process.