摘要
采用微波辐射法改性β分子筛,并将改性后的分子筛(Hβ)用于催化乙苯与苯酐一步法合成乙基蒽醌,探究了Hβ分子筛的再生及反应混合物的分离提纯方法.结果表明:改性β分子筛的最适宜条件为微波辐射加热功率390W,加热时间15min,干燥功率325W,干燥时间20min,氢交换次数为一次;分子筛先采用微波干燥,再于550℃焙烧5h后催化活性最好,一次再生后催化性能可恢复到新分子筛的92%;产物分离提纯过程中先采用石油醚将产物和未反应的苯酐分离,再用异丙醇进行重结晶效果最好,纯度可超过99%,回收率达到92%.
The β zeolite is modified over microwave radiation method. These modified zeolites（Hβ）are used to catalyze the one-step reaction of ethyl benzene with phthalic anhydride to afford ethyl anthraqui- none, the regeneration of HI3 zeolites and the separation and purification of products are studied. It is show that the optimum conditions are as follows： the heating power of the microwave radiation is 390 W, the heating time of the microwave radia drying time of microwave radiation is on 20 is 15 min; the drying power of microwave radiation is 325 W, min, H-exchange times is 1. When the zeolite is calcined at 550℃ for 5 h before dried by microwave radiation,it possesses the best the catalytic activity. The catalytic activity can be recovered to 92% of the fresh zeolite afte the first regeneration. This study found that ethyl anthra- quinone and unreacted phthalic anhydride are isolated over petroleum ether. Then pure products are obtained by recrystallization in isopropanol. The purity rate of ethyl anthraquinone is above 99% with a yield of 92%.
作者
刘为清
贾丹丹
张兴刚
姜翠玉
LIU Wei-qing JIA Dan-dan ZHANG Xing-gang JIANG Cui-yu(Periodical Office of China University of Petroleum College of Chemical Engineering in China University of Petroleum College of Science in China U＇niversity of Petroleum, 266580, Qingdao, Shandong, PRC)
出处
《曲阜师范大学学报（自然科学版）》
CAS
2017年第4期89-94,共6页
Journal of Qufu Normal University(Natural Science)
关键词
HΒ分子筛
再生
提纯
微波辐射法
乙基蒽醌
Hβ zeolite
regeneration
purification
microwave radiatione
ethyl anthraquinon
