Keggin型Ni/Cu/2,2'-联咪唑-钨硅酸盐催化合成环己酮乙二醇缩酮  

Synthesis of cyclohexanone ethylene ketal catalyzed by Keggin-type Ni / Cu /2,2'-H_2 biim-tungstosilicates

作　　者：朱再明[1] 王宇[1] 玉占君[1] 王秋雪[1] 都京 苏芳[1] 

机构地区：[1]辽宁师范大学化学化工学院,辽宁大连116029

出　　处：《应用化工》2015年第5期882-886,889,共6页Applied Chemical Industry

基　　金：辽宁省自然科学基金(2013020128);辽宁省教育厅科学研究基金(L2013414);辽宁师范大学青年基金(2014)

摘　　要：以Keggin型钨硅酸为母体化合物,利用直接沉淀法将2,2'-联咪唑(H2biim)、Ni2+、Cu2+及其联咪唑配合物引入多金属氧酸盐(POM)中,合成了Keggin型Ni/Cu/H2biim-钨硅酸盐系列化合物。通过单晶X-射线衍射、红外光谱(IR)和元素分析等手段对所合成的化合物进行了表征。以催化环己酮与乙二醇反应合成环己酮乙二醇缩酮为模型反应,研究探讨了该系列钨硅酸盐的催化性能。结果表明,大的抗衡离子引入减小了POM的溶解性,催化剂可回收重复使用,提高了催化剂的利用率。该系列钨硅酸盐非均相催化剂,经3次循环使用后,其催化活性几乎不变。A series of Keggin-type Ni/Cu/H2biim-tungstosilicates （ H2biim = 2,2＇-biimidazole） were syn- thesized with the parent tungstosilicacid as a reactant and H2biim,Ni2 ＋/Cu2＋ and their complexes as raw materials by a direct precipitation method. They were characterized by single crystal XRD, IR and elemen- tal analysis. The acid-catalyzed synthesis of cyclohexanone ethylene ketal by the reaction of cyclohexanone with ethylene glycol was selected as a model reaction. The catalytic activities of these tungstosilicates were investigated. The results show that the introduction of large cation reduced the POM＇ s solubility, and the catalysts can be recycled and reused, so that their utilization can be improved. Moreover, the catalytic ac- tivities of these heterogeneous catalysts were almost unchanged after three cycles.

关 键 词：KEGGIN结构 多金属氧酸盐 钨硅酸盐 酸催化 

分 类 号：TQ032.4[化学工程] O614[理学—无机化学]