摘要
采用气相色谱-质谱联用(GC-MS)技术,对工业级正辛基二茂铁原料组成进行分析,相对纯度仅为90.00%,其中的杂质主要为二茂铁的同系物与同分异构体。在此基础上,以正辛基二茂铁的收率及气相色谱法分析提纯产物中正辛基二茂铁的相对含量为指标,对减压蒸馏、柱层析及重结晶等几种分离工艺进行初探,最后采用混合溶剂进行低温、多次重结晶对工业级正辛基二茂铁进行有效提纯;对重结晶的溶剂混合比、重结晶的温度、时间、次数进行了优化:混合溶剂乙酸乙酯、甲醇、正己烷的体积比依次为2∶2∶5,结晶温度零下50℃,结晶时间4 h,结晶次数6次,得到纯度、收率较高的正辛基二茂铁。用气相色谱法和核磁共振定量法分析表明最终产物中正辛基二茂铁的相对纯度大于99.50%,回收率为73.0%。
The components of industrial grade n-octylferrocene were analyzed by gas chromatography-mass spectrometry（ GCMS）,and the purity of n-octylferrocence is only 90.00%. The main impurities are some homologs and isomers of ferrocene. With the relative content and recovery of product as index of purification,several methods were utilized to separate and purify n-octylferrocene,such as vacuum distillation,column chromatography,and recrystallization. The results show that the most effective method is recrystallization under a mixed solvent after several times at low temperature. The recrystallization condition： crystallization solvent,blended solvent ratio,crystallization temperature and time,as well as times of crystallization were investigated in detail. The results show that the higher purity of n- octylferrocene can be obtained under blended solvent ratio（ ethyl acetate： methanol： hexane =2 ∶ 2 ∶ 5（ volume））,along with 6 times recrystallization at minus 50 ℃. The final purity is determined by gas chromatography（ GC） and H-nuclear magnetic resonance（1HNMR）,which is over 99.50%,and the recovery is 73.0%.
出处
《固体火箭技术》
EI
CAS
CSCD
北大核心
2016年第4期524-528,共5页
Journal of Solid Rocket Technology
基金
国防技术基础科研项目(科工技[2012]1481号)
关键词
正辛基二茂铁
重结晶
分离
提纯
优化
n-octylferrocene
recrystallization
separation
purification
optimization
