【摘要】 研究了尿素-氯化胆碱DES中由均苯四甲酸二酐制取均苯四甲酸二酰亚胺工艺,考察了反应时间、反应温度及DES与均苯四甲酸二酐PMDA比例对产物收率的影响,通过响应面实验和Design-Expert中岭回归分析对反应条件进行了优化,得出最佳反应温度为130℃、反应时间4 h、DES与均苯四甲酸二酐质量比8.1:1,最终产物收率可达93.0%。采用红外光谱、紫外-可见光光谱仪、熔点仪、XRD对合成产物进行了表征,证明产品为均苯四甲酸二酰亚胺。基于尿素-氯化胆碱低共熔溶剂分解动力学,提出了简单的反应机理。尿素-氯化胆碱DES可起到溶剂、原料兼催化剂三重作用,且可重复使用,实现了均苯四甲酸二酰亚胺的绿色合成。更多还原

【Abstract】 The preparation process of pyromellitic diimide by pyromellitic dianhydride in urea-choline chloride deep eutectic solvent(DES) was explored.The effects of reaction time,reaction temperature and mass ratio of DES and pyromellitic dianhydride PMDA on product yield were investigated.The reaction conditions were optimized by response surface experiment and Design-Expert midrange regression analysis.The results showed that the reaction temperature was 130 ℃,the reaction time was 4h,the mass ratio of DES to pyromellitic dianhydride was 8.1:1,and the yield of the final product could reach 93.0%.The product was characterized and was confirmed by infrared spectrum,UV-visible light spectrometer,melting point analyzer and XRD.Meanwhile,a possible reaction mechanism was proposed and a kinetic model for the decomposition of urea-choline chloride DES was established.Ureacholine chloride DES played a triple role of solvent,reactant and catalyst,and could be reused,suggesting that the green synthesis of pyromellitic diimide was achieved.更多还原