摘要
以ω-腈基十一酸（11-CUA）的收率及纯度为目标函数，对三种分离提纯1，1′-过氧化双环已胺裂解所得油水混合物中的11-CUA的工艺进行了对比实验，确定了合适的分离提纯工艺，采用单因素实验与正交试验优化了分离提纯的工艺条件。实验结果表明，合适的分离提纯工艺为：先将裂解产物用氨水（或氨气）氨化、有机溶剂萃取，然后用硫酸（或盐酸）酸化11-CUA铵盐水溶液、再将粗品11-CUA于合适介质中结晶，得到高纯度11-CUA晶体；优化工艺条件为：氨化pH值8．0～10．0、温度25-35℃，甲苯为萃取剂，酸化pH值1．5～2．0、温度55-60℃，环己烷为结晶介质，粗品11-CUA在环己烷中溶解温度50～55℃、与环己烷初始质量比4：100、结晶前沉降分层时间10min、结晶温度20℃。采用上述工艺及工艺条件分离提纯11-CUA，产品纯度达99．90％、收率90．22％。
Taken the purity and recovery rate as object, three different self-designed separating and purifying processes used to obtain ω-cyanoundecanoic acid （11-CUA） from the oil and water mixture produced from the 1, 1＇-peroxydicyclohexylamine （PXA） pyrolysis were compared, and the most suitable one of them was chosen. The selected process consists of several steps as follows. Firstly, ammonifying the oily mixture of PXA pyrolysis by ammonia or aqueous ammonia, then adding the organic solvent to extract the impurities in the ammonified mixture secondly, acidifying the water layer of the ammonified mixture containing cyanoundecanoate by sulfuric or hydrochloric acid to obtain the crude 11-CUA thirdly, and finally, crystallizing it in suitable medium to yield high purity 11-CUA crystals. The technological parameters of the selected process were optimized by single factor experiments and orthogonal tests respectively. The results show that the optimized parameters of the process are as follows. The pH value and temperature used for ammonifying are 8.0-10.0 and 25-35℃ respectively, toluene is chosen as extraction solvent, the pH and temperature used for acidifying are 1.5-2.0 and 55-60℃ respectively, cyclohexane is selected as crystallization medium and the crude 11-CUA is dissolved at 50-55℃, initial mass ratio of crude 11-CUA to cyclohexane is 4 ： 100, demixion time of cyclohexane solution of 11-CUA before crystallizing is 10 minutes and crystallization temperature is 20℃. Using above mentioned selected process and the optimized process parameters, the 11-CUA product purity and recovery rate can reach 99.90% and 90.22%, respectively.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2007年第1期150-154,共5页
Journal of Chemical Engineering of Chinese Universities
基金
湖南文理学院科研项目(JJYB0508)
关键词
ω-腈基十一酸
分离
提纯
工艺
ω-cyanoundecanoic acid
separation
purification
process
