一种由甘油合成1,3-丙二醇的路线研究

以甘油为原料经氯代、环化、加氢反应3步合成了1,3-丙二醇。较优的反应条件为:氯代反应在醋酸(质量分数为6%)为催化剂、温度90℃反应3.5 h;环化反应在n(3-氯-1,2-丙二醇)∶n(氢氧化钠)=1∶1、氢氧化钠的质量分数为40%、温度为0℃反应1.5 h;加氢反应在钴-氧化镁/硅胶作催化剂、n(氢气)∶n(环氧丙醇)=10∶1、环氧丙醇的质量分数为20%、温度为100~150℃反应4 h;1,3丙二醇的总产率可达58.6%。

Study on synthesis process of 1,3-propanediol from glycerol

1,3-Propanediol is synthesized from glycerol by chloration,cyclization and hydrogenization.The structure of the target compound is determined by IR and 1H-NMR.The optimal reaction conditions are shown as follows:chloration at 90℃ for 3.5 hours with 6%(by mass) acetic acid as catalyst,cyclization at 0℃ for 1.5 hours with 1∶1 of the ratio of 3-chloro-1,2-propanediol and sodium hydroxide(40% by mass),and hydrogenization catalyzed by Co-MgO/silica gel at 100～150℃ for 4 hours with 10∶1 of the ratio of H2 and glycido(20% by mass).The overall yield of the reactions is 58.6%.