1,6-己二醛合成工艺研究

根据环己烯分子结构特点及相关反应的基础理论,提出在甲酸作为载氧剂的条件下,以过氧化氢氧化环己烯制备反式-1,2-环己二醇的工艺路线;并使用高碘酸钠/硅胶体系氧化反式-1,2-环己二醇制备1,6-己二醛.通过单因素实验法对在合成过程中的物料配比、反应温度、反应时间、重结晶方法等诸多因素对反应的影响进行考察.以气相色谱对产品纯度进行分析,得出反式-1,2-环己二醇及1,6-己二醛的纯度分别为98.93%和99.97%,并利用GC、红外光谱、核磁共振等分析方法对其产品化学结构进行确认.

Study on Synthesis of 1,6-Hexanedial

According to the structure of cyclohexene and correlative synthesis theory, the method of synthesizing trans-1,2-cyclohexanediol was found, which was using hydrogen peroxide to oxidize cyclohexene to the target product while the formic acid was existing as oxygen carrier. And then the 1,2-cyclohexanediol which has been made can be oxidized to 1,6-hexanedial in the oxidation system with sodium periodate/ silica gel. The factors influencing on synthesizing 1,2-diol and 1,6-hexanedial, such as raw materials ratio, reaction temperature, reaction time, the method of crystallization, etc ,were investigated with the help of the single-factor-experiment. And the purities of 1,2-cyclohexanediol and 1,6-hexanedial were analyzed by GC. They were respectively 98.926% and 99.965%. Then the structure of the products were confirmed by GC, IR and ~1HNMR.