【作者】 汪琛；

【导师】 袁其朋；

【作者基本信息】 北京化工大学 ， 制药工程， 2007， 硕士

【摘要】 研究异氰酸酯封闭技术对于促进异氰酸酯深度开发,具有重要意义。作为橡胶胶粘剂使用的封闭异氰酸酯要求其解封闭温度低于250℃,且封闭效力高,常温保存稳定性好。在众多异氰酸酯封闭剂中ε-己内酰胺的解封闭温度较低,价廉易得,基本上不存在污染问题。因此,对ε-己内酰胺封闭的异氰酸酯反应条件进行了研究。首先,研究了ε-己内酰胺封闭4,4’-二苯甲烷二异氰酸酯(MDI)反应的各个影响因素,详细讨论了封端反应的加料方式、加料时间、催化剂用量、反应温度、原料物质的量配比、反应时间、搅拌速度、溶剂的选择各个因素对反应过程的影响。并通过正交实验,优化了反应条件。其次,探索了亚硫酸氢钠提纯粗产品的工艺。通过对反应温度、溶剂因素的考察分析,优化了提纯工艺。用高效液相分析了处理前后产品的纯度。再次,用熔点测定、薄层层析定性验证了产物质量。通过质谱(ESI)、核磁和气质联机分析,证实了产物的结构。通过热重分析(TG-DSC),测定了产品分解温度,为184.1℃,并且证实了产品在室温下长时间放置的稳定性好。最后,用红外、气质联机、ESI质谱等仪器成功地对国外产品进行了剖析,了解国外产品的配方,并尝试进行了复配。更多还原

【Abstract】 The isocyanate blocking technology is of great significance to further development and application of isocayanate adhesives. The blocked isocyanate adhesives that applied as rub adhesive should be unblocked under less than250℃, and the good blocking ability and good storage at room-temperature are demanded of abundant blocking agents, the e-caprolactam has special properties such as low unblocking temperature, low price and almost no pollution. So conditions of diblocking reaction between ε-caprolactam and Diphenylmethane-4,4’-Diisocyanate (MDI) was studied.Firstly, blocking reaction of MDI with ε-caprolactam were well investigated, which included the route and sequence of addition of reactants, dosage of catalyst, temperature, raw material ratio, reaction time, stirring speed and solvent. The choice of reaction conditions was based on a Latin Square design.Secondly, it also well discussed the blocking technology of crude product with sodium bisulfate and the effect of each technological paramaters on the purification reaction such as reaction temperature and solvent. The purification technology for cude product was optimized. Meanwhile the purity of the treated product and crude product was analyzed by HPLC.Thirdly, the purity of the treated product was analyzed by melting point and TLC. The structure of the treated product is identified by ESI-MS, NMR and GC-MS. The thermal decomposition temperature of the purified production was184.1℃, measured by TG-DSC. It is well proved that a good ability of storage at room temperature.Finally, imported product was successfully analyzed by FTIR, GC-MS, ESI-MS. The ingredient of imported product was recognized. Imitating foreign product has been tried.更多还原