Study On Separation And Purification Process Of Effective Components From Anise Oil

In view of conditions in deep processing technology of anise oil,separation and purification process of trans-anethole was optimized,and separation and purification process of estragole by vacuum batch distillation was explored and researched in the study.The following four aspects were included in the study.1.The anise oil was analyzed by GO/MS.Its main components were trans-anethole(76.08%),estragole(7.73%),acetone anethole(4.15%),α,β-ph-ellandrene(1.29%),linalool(2.31%),caryophyllene(1.03%),α,β-pinene(0.71%),cis-anethole(0.67%),anisic aldehyde(0.65%),and low content of terp-enoids.2.Making anise oil as raw material,process conditions of separation and purification of trans-anethole in freezing crystallization was researched.Crystallization temperature and crystallization time were researched on the yield and purity of trans-anethole,and the process was optimized.Expe-riment results showed the optimized conditions were as follow:crystalliz-ation time was 4 h,crystallization temperature was 5℃.Under the cond-itions,the purity of trans-anethole was 94.81%,its yield was 79.49%.By GC/MS,the most of terpenoids in the crude anethole after separated was removed,its main components were trans-anethole(94.81%),cis-anethole(0.55%),linalool(0.11%),estragole(0.72%),anisic aldehyde(0.53%),acetone anethole(0.12%).3.Making anethole separated from anise oil by freezing crystallization as raw material,the total reflux time,reflux ratio and operational pressure on the separation effects of light components(linalool,estragole)and trans-anethole were researched by single factor test in vacuum batch distillation,and the process was optimized.The optimized process was as follow:when the vacuum was not less than 93.33 kPa,after total reflux time of 1 h,products were attained at a reflux ratio of 1:1.The purity of trans-anethole was 99.7%and its yield was 78.45%.4.Making 81%of estragole enriched as raw material,the reflux ratio and operational pressure on the separation effects were respectively explored in two-step vacuum batch distillation,and the process was optimized.The optimized process was as follow:in the first step,when the vacuum was 91.99 kPa,after total reflux time of 1 h,light component(linalool)were attained at a reflux ratio of 10:1;in the second step,when the vacuum was 91.99 kPa,after total reflux time of 1 h,products were attained at a reflux ratio of 6:1.With two-step variable reflux ratio operation,the reflux ratio from 10:1 to 6:1,the purity of estragole was 98.69%and its yield was 72.46%.