摘要
采用多变参数间歇精馏技术对四甲基哌啶酮粗品进行了提纯实验研究。色谱分析证明,得到的哌啶酮产品质量分数达98.6%以上,一次收率超过64%;复蒸2#馏出物后得到的塔顶产品经过色质联用分析后确定为4-甲基-3-戊烯-2-酮及同分异构体4-甲基-4-戊烯-2-酮的混合物,其中4-甲基-3-戊烯-2-酮质量分数达88%以上。
This paper deals with the vacuum batch distillation experiment by the multivariable parameters' strategy for rectifying the crude 4-piperdinone generated from the reaction of acetone with liquid ammonia. Gas chromatographic analysis shows that the purity of the 4-piperidinone product obtained by batch distillation was more than 98.6% and its first yield was over 64%. And the by- product,the mixture of 4-methyl-3-pentene-2-one and 4-methyl-4-pentene-2-one, which was produced from the same reaction, was enriched to over 88% ( by GC-MS ). The experiment shows that it is viable to rectify 4-piperdinone. by distillation instead of re-crystallization which is a much longer separation process and a more complicated job.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2011年第12期1188-1190,1198,共4页
Fine Chemicals