微波辐射促进P_2O_5催化液相贝克曼重排制己内酰胺  

Microwave Radiation Promoted Liquid-Phase Beckmann Rearrangement of Cyclohexanone Oxime for Preparing ε-Caprolactam Over P_2O_5 Catalyst

作　　者：程庆彦[1] 姬亚宁[1] 王延吉[1] 

机构地区：[1]河北工业大学绿色化工研究所,天津300130

出　　处：《石油学报（石油加工）》2011年第3期393-398,共6页Acta Petrolei Sinica(Petroleum Processing Section)

基　　金：国家自然科学基金(20906018);河北省自然科学基金(B2010000016);河北省教育厅科学研究计划项目(2009428)资助

摘　　要：在微波辐射的条件下,以P2O5为催化剂,开发了液相贝克曼重排制己内酰胺(CPL)的新型工艺。研究了加热方式、催化剂(H3PO4、ZnCl2和P2O5)、反应容器、微波辐射强度、辐射时间、催化剂用量以及溶剂(环己酮、水和N,N-二甲基甲酰胺)对环己酮肟液相贝克曼重排反应的影响。在催化剂P2O5的质量分数为14.0%(0.19 g)、10 mLN,N-二甲基甲酰胺为反应介质、1.153 g环己酮肟、微波辐射强度为280 W、辐射时间为5.0 min的工艺条件下,环己酮肟的转化率能达到98.69%,己内酰胺收率达到95.75%。此外,该工艺操作简单,反应迅速,收率较高,具有潜在的工业化应用前景。The new technology of Beckmann rearrangement of cyclohexanone oxime was effectively developed to prepare ε-caprolactam（CPL） over P2O5 catalyst under microwave radiation.The effects of the heating method,catalyst（H3PO4,ZnCl2 and P2O5）,reactor,power of microwave radiation,time of microwave radiation,mass capacity of P2O5,solvent（cyclohexanone,water and N,N-dimethyl formamide） on cyclohexanone oxime rearrangement reaction were investigated.The cyclohexanone oxime conversion of 98.69% and ε-caprolactam yield of 95.75% was obtained when the reaction was carried out under the conditions of 10 mL N,N-dimethyl formamide,P2O5 0.19 g and cyclohexanone oxime 1.153 g at 280 W microwave radiation power for 5.0 min.At the same time,this method has advantage of simple operation,rapid reaction,high yield and potential industrial application prospects.

关 键 词：己内酰胺(CPL) P2O5催化剂 微波辐射 液相贝克曼重排 

分 类 号：TQ340.69[化学工程—化纤工业]