胺化改性磺酸型阳离子交换树脂酸碱协同催化环己酮自缩合反应  

Self-Condensation of Cyclohexanone Catalyzed with Amine Modified Sulfonie Acid Ion Exchange Resins

作　　者：徐斌[1] 刘艳秋[2] 王俊格[2] 任晓乾[2] 马文明[2] 武文良[2] 

机构地区：[1]南京工业大学理学院 [2]南京工业大学化学化工学院,江苏南京210009

出　　处：《高校化学工程学报》2015年第2期335-340,共6页Journal of Chemical Engineering of Chinese Universities

基　　金：材料化学工程重点实验室开放项目;国家重点基础研究规划(973计划)资助项目(2009CB724701)

摘　　要：采用乙二胺对磺酸型阳离子交换树脂进行胺化改性,并运用CHNS元素分析及傅里叶变换红外光谱对改性树脂进行了表征。结果表明,胺化改性后树脂含氮量为0.94 mmol?g?1,改性后树脂骨架结构变化不大,胺基成功固载到树脂上,碱性增强,使氢型树脂成为具有酸碱双功能的催化剂。在催化环己酮缩合反应中考察了胺化量、催化剂用量、反应温度、反应时间、带水剂种类及用量等条件对反应的影响。实验结果表明,以甲苯为带水剂效果较好。在5%(wt)胺化量改性树脂,10%(wt)催化剂用量,7 m L甲苯为带水剂,120℃反应3 h的优化条件下,环己酮转化率为62.1%,二聚物选择性98.0%,体现出了酸碱协同催化环己酮缩合反应优异性能。改性树脂重复使用5次后,催化性能仍较稳定。Sulfonie acid ion exchange resins were modified with ethylenediamine and characterized by FTIR and CHNS elemental analysis. The results show that resins with 0.94 mmol·g^-1 nitrogen were obtained through amine modification. Moreover, the skeleton structure of the modified resin does not change and its basicity is strengthened to become an acid-base bifunctional resin catalyst. Effects of catalyst dosage, reaction temperature, reaction time, water carrier variety and dosage on self-condensation of cyclohexanone were investigated. Toluene was chosen as a good water carrier. Under optimum conditions（amination rate 5%（wt）, catalyst dosage 10%（wt）, toluene dosage 7m L, reaction time 3 h and reaction temperature 120℃）, conversion of cyclohexanone and selectivity of dimer product are 62.1 % and 98.0 %, respectively. Furthermore, the modified resin shows good reusability after using for 5 times.

关 键 词：磺酸型离子交换树脂 胺化 酸碱双功能 环己酮 缩合 

分 类 号：TQ032.41[化学工程]