Environment-friendly synthesis of N-phenylpiperidine from aniline and 1,5-pentanediol overγ-Al_2O_3 catalyst

An efficient environment-friendly synthesis of N-phenylpiperidine was developed from aniline and 1,5-pentanediol over γ-Al2O3 catalyst under atmospheric pressure. The conversion of 1,5-pentanediol reached 97% and the selectivity for N-phenylpiperidine attained 94%. The structure of the catalyst was characterized by NH3-TPD and BET. The influences of calcination temperature of the catalyst and reaction temperature on activity and selectivity of the catalyst were investigated.

甲醇钠催化合成2,2,4-三甲基-1,3-戊二醇单异丁酸酯

研究了合成2,2,4-三甲基-1,3-戊二醇单异丁酸酯的新工艺。以异丁醛为原料,甲醇钠为催化剂,由一段反应工艺实现醇醛缩合、坎尼扎罗两步反应生成目标产物,较好的反应条件为:催化剂用量4g甲醇钠/(200g异丁醛),反应温度60℃,反应时间4h,使得异丁醛的单程转化率达到80%以上,目标产物的选择性达到97%以上。

十二碳醇酯的合成与同分异构体的调控

以异丁醛为原料,通过两种不同的工艺催化合成十二碳醇酯,并可以在一定范围内对合成的醇酯十二同分异构体含量进行调控(伯酯/仲酯为1.38~1.86)。优化了一步法合成的工艺条件:催化剂采用BaO,质量分数为7%,反应温度为50℃,反应时间为30min。反应转化率达84.2%,选择性达98%。采用GC、~1H NMR对产物及同分异构体组成进行分析表征,并将得到的不同同分异构组成的样品进行成膜性能测试。结果表明,实验成功调控制备了不同同分异构组成的十二碳醇酯,伯酯含量较高的成膜性能较好。