论文部分内容阅读
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%。
Glycerol was used as raw material, and after 4 generations of chlorination, oxidation, Clementon reduction and hydrolysis, the 1,3-propanediol was finally synthesized and the structure of the target product was confirmed by infrared spectroscopy and mass spectrometry. The reaction conditions are optimized from the reactant molar ratio, the reaction temperature, the reaction solvent and the like. The optimal reaction conditions were as follows: chlorination reaction: temperature 120 ℃; oxidation reaction temperature 23-27 ℃, n (1,3-dichloro-2-propanol) The amount of reaction solvent: 1 mL of water to dissolve 1.4 g of 1,3-dichloro-2-propanol; Clemson reduction: n (1,3-dichloroacetone) As the optimum reaction solvent, under this condition, the yield of 1,3-propanediol can reach 37.1%.