摘要
选取乙醇、甲苯、丙酮、乙醚4种溶剂对顺,反,顺-1,2,3,4-环丁烷四甲酸二酐粗品(简称CBDA)进行洗涤,抽滤、恒温干燥、重结晶后得到纯度较高的CBDA产品。分析讨论了洗涤次数和4种有机溶剂对产品纯度的影响,通过验证性实验确定出CBDA提纯工艺条件为:溶剂为无水乙醇,溶剂配比为1:5,搅拌时间为30mim(常温),4次洗涤,乙酸酐回流2h。高效液相色谱分析了提纯后的产品纯度为99.18%。
High purity products is obtained by washing, filtration, Constant temperature drying, recrystallization to cis, trans, eis - 1,2,3,4 - Cyclobutanetetraearboxylic Dianhydride crude (CBDA) with four kinds of solvent solu- tion such as Ethanol, Toluene, Acetone, Ether. It discussed the impact of the number of washing and four kinds of organic solvents on product purity, determined CBDA purification conditions by validation experiments. The condi- tion is:solvent is ethanol, solvent ratio is 1:5, stirring time is 30mim( normal temperature), Acetic Anhydride is refluxed for 2h,the solvent was washed four times. Product purity of CBDA purified by HPLC is 99.18%.
作者
凌洁
LING Jie(Department of Chemical Engineering, Shaanxi Energy Institute, Xianyang 71200, Chin)
基金
陕西省教育厅专项科学研究项目(16JK1168).
关键词
环丁烷四甲酸二酐
液相色谱
提纯
Cyelobutanetetracarboxylic dianhydride
liquid chromatography (HPLC)
purify