在1-丁基-3-甲基咪唑四氟硼酸盐([bmim][BF4])与甲苯组成的两相体系中,以三氯化磷(PCl3)为催化剂,实现了由环己酮肟制备己内酰胺的液相贝克曼重排反应,两相体系有利于反应控制和体系取热.研究了环己酮肟用量、PCl3用量、反应时间和反应...在1-丁基-3-甲基咪唑四氟硼酸盐([bmim][BF4])与甲苯组成的两相体系中,以三氯化磷(PCl3)为催化剂,实现了由环己酮肟制备己内酰胺的液相贝克曼重排反应,两相体系有利于反应控制和体系取热.研究了环己酮肟用量、PCl3用量、反应时间和反应温度对重排效果的影响.优化反应条件为:2 ml[bmim][BF4],5 ml甲苯,0.3 ml PCl3,5 ml 2 mol/L环己酮肟-甲苯溶液,90℃,反应时间10～30 min.此时,环己酮肟转化率达98.96%,生成己内酰胺的选择性达87.30%,PCl3催化转化数达2.88.生成的大部分己内酰胺在离子液体相.展开更多
Recovery of caprolactam from waste water of caprolactam production factory was investigated using benzene as solvent in a small-scale pulsed-sieve-plate column. First, liquid-liquid equilibrium (LLE) data were measure...Recovery of caprolactam from waste water of caprolactam production factory was investigated using benzene as solvent in a small-scale pulsed-sieve-plate column. First, liquid-liquid equilibrium (LLE) data were measured, including water-caprolactam-benzene system at low caprolactam concentrations, and waste water-benzene system. Then, the operating regions and mass transfer of the pulsed-sieve-plate column were measured. Finally, the overall apparent heights of a transfer unit based on continuous phase are correlated in terms of the column operation variables.展开更多
A simple and efficient approach for the synthesis of e-caprolactam via the liquid phase nitrosation of cyclohexane and nitrosyl sulfuric acid in the presence of concentrated sulfuric acid has been developed. A series ...A simple and efficient approach for the synthesis of e-caprolactam via the liquid phase nitrosation of cyclohexane and nitrosyl sulfuric acid in the presence of concentrated sulfuric acid has been developed. A series of novel A1VPO composites were prepared by an impregnation method and the composites were then employed to catalyze the nitrosation reaction of cyclohexane and nitrosyl sulfuric acid. Compared to the reaction using fuming sulfuric acid, the selectivity for the desired product was significantly improved using this one-step catalytic process. This method affords a shortcut to prepare ecaprolactam and its analogs from cyclohexane.展开更多
文摘在1-丁基-3-甲基咪唑四氟硼酸盐([bmim][BF4])与甲苯组成的两相体系中,以三氯化磷(PCl3)为催化剂,实现了由环己酮肟制备己内酰胺的液相贝克曼重排反应,两相体系有利于反应控制和体系取热.研究了环己酮肟用量、PCl3用量、反应时间和反应温度对重排效果的影响.优化反应条件为:2 ml[bmim][BF4],5 ml甲苯,0.3 ml PCl3,5 ml 2 mol/L环己酮肟-甲苯溶液,90℃,反应时间10～30 min.此时,环己酮肟转化率达98.96%,生成己内酰胺的选择性达87.30%,PCl3催化转化数达2.88.生成的大部分己内酰胺在离子液体相.
基金Partly supported by UK's Academic Link with China Scheme (ALCS: SHA/992/307), British Council.
文摘Recovery of caprolactam from waste water of caprolactam production factory was investigated using benzene as solvent in a small-scale pulsed-sieve-plate column. First, liquid-liquid equilibrium (LLE) data were measured, including water-caprolactam-benzene system at low caprolactam concentrations, and waste water-benzene system. Then, the operating regions and mass transfer of the pulsed-sieve-plate column were measured. Finally, the overall apparent heights of a transfer unit based on continuous phase are correlated in terms of the column operation variables.
文摘A simple and efficient approach for the synthesis of e-caprolactam via the liquid phase nitrosation of cyclohexane and nitrosyl sulfuric acid in the presence of concentrated sulfuric acid has been developed. A series of novel A1VPO composites were prepared by an impregnation method and the composites were then employed to catalyze the nitrosation reaction of cyclohexane and nitrosyl sulfuric acid. Compared to the reaction using fuming sulfuric acid, the selectivity for the desired product was significantly improved using this one-step catalytic process. This method affords a shortcut to prepare ecaprolactam and its analogs from cyclohexane.
