洗油甲基萘馏分中喹啉盐基的回收与提纯  

Recovery and purification of quinoline base in methyl naphthalene fraction of wash oil

作　　者：赵明[1] 辛燕平[1] 李汇丰 焦红普[1] 许春建[1] 

机构地区：[1]天津大学化学工程联合重点实验室,天津300072 [2]河南宝舜化工科技有限公司,河南安阳455000

出　　处：《化学工程》2013年第8期6-10,15,共6页Chemical Engineering(China)

摘　　要：喹啉盐基指沸点160—270℃、主要存在于洗油甲基萘馏分中的喹啉、异喹啉及其衍生物。文中建立了甲基萘馏分及喹啉盐基的气相色谱分析方法,解决了甲基萘馏分中主要组分的定性和定量分析问题。通过单级萃取实验,得到了从甲基萘馏分中萃取喹啉盐基的优化操作条件:硫酸为萃取剂,硫酸铵为稀释剂,萃取剂质量分数10%,稀释剂质量分数10%,萃取温度为室温,萃取时间15 min。为提高喹啉盐基的萃取率,采用单级萃取最佳工艺条件,对连续逆流反应萃取实验进行研究,重点考察重相进料流速对萃取率的影响。结果表明:当重相进料流速低于液泛速度时,萃取率达(质量分数)99.9%以上。通过间歇蒸馏实验,对粗喹啉盐基进行了精制,得到了纯度质量分数99%以上的精喹啉盐基产品。文中介绍的提取喹啉盐基的方法具有易实现、工序少、工艺简单和收率高的优点。Quinoline base mainly refers to quinoline, isoquinoline and their derivatives with the boiling point of 160--270℃, mainly existing in the methyl naphthalene fraction of wash oil. The gas chromatography analysis method for methyl naphthalene fraction and quinoline base was established, thus solving the problem in analyzing the main components in the methyl naphthalene fraction qualitatively and quantitatively. Through the single-stage extraction experiments, the optimum extraction conditions were obtained by the selection experiments： sulfuric acid as extraction agent, ammonium sulfate as diluent, extractant mass fraction of 10%, diluent mass fraction of 10%, extraction at room temperature, extraction time of 15 min. In order to improve the extraction rate of the quinoline base, using single-stage extraction optimum conditions, the continuous countercurrent reactive extraction was investigated, focusing on the effects of the heavy-phase feed flow rate on the extraction rate. The result shows that the extraction rate is above 99.9% when the heavy-phase feed flow rate is less than the flooding velocity. The crude quinoline base was refined by batch distillation, and the pure quinoline base product with the mass fraction of 99% was obtained. The method of extracting quinoline base described has the advantages of easy realization, less process steps, simple process and high product yield.

关 键 词：喹啉盐基 反应萃取 萃取塔 间歇蒸馏 

分 类 号：TQ028.94[化学工程]