甘油合成1,3-丙二醇

以甘油为原料,经过氯代、氧化、克莱门森还原、水解4步反应,最终合成1,3-丙二醇,并用红外光谱仪和质谱仪对目标产物进行结构确定。从反应物摩尔比、反应温度、反应溶剂等优化了反应条件。最优反应条件为:氯代反应:温度120℃;氧化反应:温度23～27℃,n(1,3-二氯-2-丙醇)∶n(重铬酸钠)=1.8∶1,反应溶剂用量:1 mL水溶解1.4 g 1,3-二氯-2-丙醇;克莱门森还原反应:n(1,3-二氯丙酮)∶n(锌)=1∶1.2,水作反应溶剂最佳,在该条件下,1,3-丙二醇总产率可达37.1%。

Synthesize of 1, 3-propanediol from glycerol

1,3-Propanediol was synthesized from glycerol by chloration,oxidation,Clemmensen reaction and hydrolysis.The structure of the target compound was determined by method of IR and MS.The molar ratio,temperature and solvent of the reaction were investigated to optimize the reaction conditions.The optimum conditions are:for chloration:120 ℃;for oxidation:23～27 ℃,n(1,3-dichloroacetone)∶n(sodium dichromate)=1.8∶1,the amount of reaction solvent:1.4 g 1,3-dichloro-2-propanol per 1 mL water,and for Clemmensen reaction:n(1,3-dichloropropane)∶n(zinc)=1∶1.2,with water as the desirable solvent,and the overall yield of 37.1%.