反溶剂结晶法分离精制粗蒽的研究  

Study on separation and purification of crude anthracene by anti-solvent crystallization

作　　者：鄂永胜[1] 张元 E Yong-sheng;ZHANG Yuan(School of Biomedical and Chemical Engineering,Liaoning Institute of Science and Technology,Benxi 117004,China)

机构地区：[1]辽宁科技学院生物医药与化学工程学院,辽宁本溪117004

出　　处：《化学工程师》2022年第9期89-93,共5页Chemical Engineer

基　　金：辽宁省自然科学基金项目(20180550114);辽宁科技学院大学生创新创业训练计划项目(202111430054)。

摘　　要：采用平衡法测定蒽、菲、咔唑在溶剂DMF和乙醇中的溶解度,确定主溶剂为DMF,反溶剂为乙醇。测定蒽、菲、咔唑在不同质量比的乙醇-DMF混合溶剂中的溶解度,根据结果设计反溶剂结晶法分离精制粗蒽的方案:先用溶剂甲苯洗涤粗蒽得到半精蒽,然后用主溶剂DMF洗涤半精蒽得到部分精蒽和滤液,滤液滴加反溶剂乙醇依次结晶析出精咔唑和剩余精蒽。最优的精制条件为:M_(乙醇)∶M_(DMF)=0.6时是蒽和咔唑分离的临界点,之前析出的结晶物为精蒽,之后析出为精咔唑,结晶温度为60℃,反溶剂的滴加速度为1g·min^(-1),搅拌速度为80r·min^(-1),结晶时间1h,养晶时间1h,得到的精蒽纯度大于95%、总收率为90.05%,精咔唑纯度大于96%、收率为83%。Equilibrium method was used to determine the solubility of anthracene,phenanthrene and carbazole in the solvent DMF and ethanol.The main solvent was DMF,and the anti-solvent was ethanol.The solubility of anthracene,phenanthrene,and carbazole in ethanol-DMF mixed solvents with different mass ratios was determined.According to the data,a scheme for separating and refining crude anthracene by anti-solvent crystallization was designed:first,the crude anthracene was washed with solvent toluene to obtain semi-refined anthracene,and then the semi-refined anthracene was washed with the main solvent DMF to obtain part of the refined anthracene and the filtrate,and the filtrate was added dropwise with the anti-solvent ethanol to successively crystallize the refined carbazole and the remaining refined anthracene.The optimal refining conditions are:when Methanol∶MDMF is 0.6,it is the critical point for the separation of anthracene and carbazole,the precipitation of crystals is refined anthracene,and the subsequent precipitation is refined carbazole,the crystallization temperature is 60℃,the anti-solvent dropping rate is 1g·min^(-1),the stirring speed is 80r·min-1,the crystallization time is 1h,and the crystal growing time is 1h.The obtained refined anthracene has a purity of more than 95%and a total yield of 90.05%,the purity of refined carbazole is greater than 96%,and the yield is 83%.

关 键 词：反溶剂结晶法 分离精制 粗蒽 研究 

分 类 号：TQ420.6[化学工程]