碘催化合成对-正丁基苯胺的正交实验研究

Study on Synthesis of 4-n-Butyl Benzenamine Catalyzed by Iodine through Orthogonal Experiment

以碘作催化剂、以正丁醇与苯胺为原料在高压反应釜内催化合成对-正丁基苯胺,用GC-MS和气相色谱对产物进行定性和定量分析。通过正交实验确定最佳反应条件如下:反应温度300℃、反应时间10h、碘量0.910g(占苯胺质量的10‰)、搅拌速度450r·min-1,在此条件下,对-正丁基苯胺收率为49.84%,并在以负载型催化剂I2/Al2O3代替单质碘时达到55.51%。

4-n-Butyl benzenamine was synthesized by n-butanol and aniline with iodine as catalyst in the high-pressure reactor. The products were determined by GC-MS and GC. The optimum conditions were determined by orthogonal experiment as follows：the reaction temperature was 300 ℃,the reaction time was 10 h,iodine dosage was 0. 910 g（10‰ of mass of aniline） ,the stirring speed was 450 r ·min^-1. Under above conditions, the yield of 4-n-butyl benzenamine was 49. 84% ,and 55. 51% with I2/Al2O3 instead of iodine as catalyst.