从桉叶油母液中间歇减压精馏纯化1,8-桉叶油素  

Purification of 1,8-Cineole from Stock Solution of Eucalyptus Oil by Batch Vacuum Distillation

作　　者：王石[1] 靳林溪[1] 谢建春[1] 郑福平[1] 黄明泉[1] 孙宝国[1] 

机构地区：[1]北京市食品风味化学重点实验室,北京市食品添加剂配料工程中心,北京工商大学,北京100048

出　　处：《食品科学》2013年第8期21-26,共6页Food Science

基　　金：国家自然科学基金面上项目(31171755);北京市自然科学基金面上项目(21220213);北京市教委科技发展计划重点项目(KZ201010011011);北京工商大学研究生科研学术创新基金项目

摘　　要：研究从桉叶油工业副产品——桉叶油母液中,间歇减压精馏分离1,8-桉叶油素的工艺条件。通过绘制1,8-桉叶油素及主要杂质α-蒎烯、柠檬烯、对聚伞花烃的馏出曲线,考察塔预处理方法对精馏分离的影响。采用单因素试验和响应面分析对全回流时间、系统压力和回流比等因素进行优化,得到较佳工艺为:先乙醇洗塔-水润湿对塔进行预处理,然后精馏。精馏操作压力2.7kPa,先全回流50min后,将回流比调为2:2;当塔顶温度达60℃时,再将回流比调节至10:1;收集沸程68～73℃馏分,得1,8-桉叶油素,纯度85.1%,收率79.0%。Purification of 1,8-cineole from the stock solution produced from the industrial processing of raw eucalyptus oil was studied by batch vacuum distillation. The technique of tower packing pretreatment was selected based on effusing curves of the target 1,8-cineole as well as the main impurities of a-pinene, limonene and p-cymene in batch vacuum distillation. The effect of full-reflux time, pressure of operation system, and reflux ratio were investigated through single- factor and response surface analysis experiments. The optimum conditions for recycling of 1,8-cineole from the stock solution were obtained as follows： （1） The tower was cleaned with ethanol, and then rinsed with water; （2） Under the pressure of 2.7 kPa, the stock solution was distilled initially in a full-reflux mode for 50 min and in a reflux ratio of 2：2. When the boiling point arrived at 60 ℃, the reflux ratio was adjusted from 2：2 to 10：1 and the fraction of 1,8-cineole was then collected within the boiling point range of 68 to 73 ℃. The purity of 1,8-cineole reached up to 85.1% confirmed by GC, and the recovery was 79.0%.

关 键 词：1 8-桉叶油素 母液 桉叶油 间歇减压精馏 响应面分析 

分 类 号：TQ654[化学工程—精细化工]