应用化工
應用化工
응용화공
APPLIED CHEMICAL INDUSTRY
2015年
5期
882-886,889
,共6页
朱再明%王宇%玉占君%王秋雪%都京%苏芳
硃再明%王宇%玉佔君%王鞦雪%都京%囌芳
주재명%왕우%옥점군%왕추설%도경%소방
Keggin 结构%多金属氧酸盐%钨硅酸盐%酸催化
Keggin 結構%多金屬氧痠鹽%鎢硅痠鹽%痠催化
Keggin 결구%다금속양산염%오규산염%산최화
Keggin-type structure%polyoxometalates%tungstosilicacid%acid-catalysis
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(H2 biim)、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/ H2 biim-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。
以 Keggin 型鎢硅痠為母體化閤物,利用直接沉澱法將2,2′-聯咪唑(H2 biim)、Ni2+、Cu2+及其聯咪唑配閤物引入多金屬氧痠鹽(POM)中,閤成瞭 Keggin 型 Ni/ Cu/ H2 biim-鎢硅痠鹽繫列化閤物。通過單晶 X-射線衍射、紅外光譜(IR)和元素分析等手段對所閤成的化閤物進行瞭錶徵。以催化環己酮與乙二醇反應閤成環己酮乙二醇縮酮為模型反應,研究探討瞭該繫列鎢硅痠鹽的催化性能。結果錶明,大的抗衡離子引入減小瞭 POM 的溶解性,催化劑可迴收重複使用,提高瞭催化劑的利用率。該繫列鎢硅痠鹽非均相催化劑,經3次循環使用後,其催化活性幾乎不變。
이 Keggin 형오규산위모체화합물,이용직접침정법장2,2′-련미서(H2 biim)、Ni2+、Cu2+급기련미서배합물인입다금속양산염(POM)중,합성료 Keggin 형 Ni/ Cu/ H2 biim-오규산염계렬화합물。통과단정 X-사선연사、홍외광보(IR)화원소분석등수단대소합성적화합물진행료표정。이최화배기동여을이순반응합성배기동을이순축동위모형반응,연구탐토료해계렬오규산염적최화성능。결과표명,대적항형리자인입감소료 POM 적용해성,최화제가회수중복사용,제고료최화제적이용솔。해계렬오규산염비균상최화제,경3차순배사용후,기최화활성궤호불변。
A series of Keggin-type Ni/ Cu / H2 biim-tungstosilicates(H2 biim = 2,2′-biimidazole)were syn-thesized with the parent tungstosilicacid as a reactant and H2 biim,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.