化工进展 ›› 2016, Vol. 35 ›› Issue (02): 570-574.DOI: 10.16085/j.issn.1000-6613.2016.02.036

• 精细化工 • 上一篇    下一篇

低温控温结晶法分离提纯1,8-桉叶油素的工艺

刘文婷, 顾丽莉, 万红焱, 吕小刚   

  1. 昆明理工大学化学工程学院, 云南 昆明 650500
  • 收稿日期:2015-05-07 修回日期:2015-05-18 出版日期:2016-02-05 发布日期:2016-02-05
  • 通讯作者: 顾丽莉,教授,主要从事化学工程领域研究。E-mail:liligu001@163.com。
  • 作者简介:刘文婷(1990-),女,硕士研究生。E-mail:277388763@qq.com。
  • 基金资助:
    国家自然科学基金项目(20966004)。

Technique of low temperature control crystallization for separating and purifying 1,8-cineole

LIU Wenting, GU Lili, WAN Hongyan, LÜ Xiaogang   

  1. College of Chemical Engineering, Kunming University of Science and Technology, Kunming 650500, Yunnan, China
  • Received:2015-05-07 Revised:2015-05-18 Online:2016-02-05 Published:2016-02-05

摘要: 采用全结晶工艺对原料桉叶油[w(cineole)=63.24%]进行分离提纯,在无晶种添加下,降温速率4℃/h、结晶终温-30℃、发汗速率5℃/h、发汗终温-19℃时,可将原料油提纯至77.52%。添加晶种后,可有效提高操作温度,缩小结晶温度的操作范围,提高产品的纯度,在降温速率4℃/h、结晶终温-25℃、发汗速率4℃/h、发汗终温-6℃的操作条件下,将原料油提纯至89.63%。实验得到了低温控温添加晶种结晶法分离提纯1,8-桉叶油素的适宜工艺流程和操作参数,该方法相对其他分离方法具有较为明显的优势。

关键词: 结晶, 晶种, 1,8-桉叶油素, 速率

Abstract: A crystallization process purifying the crude Eucalyptus oil [w(cineole) = 63.24%] was studied in this paper. Without any crystal seed,the concentration of 1,8-cineole would be improved from 63.24% to 77.52% under conditions:The cooling rate was 4℃/h,the cooling final temperature was -30℃,the sweating rate was 5℃/h,the sweating final temperature was -19℃. After crystal seeds were added,the operation temperature was obviously increased,the range of crystallization temperature was effectively reduced,and the purity of the product was greatly increased. The best operating value were determined:the cooling rate was 4℃/h,the crystallization temperature was -25℃,the sweating rate was 4℃/h,the sweating final temperature was -6℃,the amount of crystal seed was 0.2%,the diameter of crystal seed was 3mm with no broken,the temperature of seed added was -17℃. Under these conditions,the purity of crude oil was increased from 63.24% to 89.63%. The suitable process and its operating parameters for separating and purifying cineole under low temperature with a little crystal seed were obtained. Compared to other separation methods,this method has obvious advantages.

Key words: crystallization, crystal seed, 1,8-cineole, rate

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