(1 辽宁大学化学科学与工程学院,沈阳 110036;
2 东北大学材料与冶金学院, 沈阳 110006)
摘 要: 采用离子交换.冷冻法制得11-钨锌合铝杂多酸[H7HAl(H2O)ZnW11O39]·12H2O。确定了反应的pH值和物料的最佳比。 用元素分析、电位滴定、红外光谱、紫外光谱、X射线粉末衍射和热分析等对合成产物进行了表征。电位滴定表明其7个质子是两步离解的。 红外光谱给出了4个特征峰, 紫外光谱给出了两个强的荷移跃迁谱带。根据X射线粉末衍射实验结果, 确认11-钨锌合铝杂多酸具有Keggin结构。 在此基础上,对其在合成己二酸二(2-乙基己)酯(DOA)中的催化性能进行了研究,其选择性为99.9%,产率为93.9%。
关键字: 11-钨锌合铝酸 杂多酸 催化剂
(1 Institute of Chemical Science and Engineering, Liaoning University, Shenyang 110036, P. R. China
2 School of Materials and Metallurgy, Northeastern University, Shenyang 110006, P. R. China)
Abstract:The undecatungstozincoaluminic heteropoly acid [H7HAl(H2O)ZnW11O39]·2H2O has been prepared by the ion exchanging-cooling method. The optimal proportion of the materials and the pH of the synthesis reaction were given. The product was characterized by elemental analysis, potentiometric titration, IR, UV, X-ray powder diffraction and thermal analysis. The potentiometric titration showed that seven protons are dissociated two-step. Four characteristic absorption peaks in IR spectrum and two intense charge-transfer bands in UV spectrum were given. According to X-ray powder diffraction determination, it was confirmed that undecatungstozincoaluminic heteropoly acid possess the Keggin structure. The catalytic performance of the heteropoly acid for etherification of 2-ethylhexyl alcohol with adipic acid was investigated. The selectivity and yield were 99.9% and 93.9%, respectively.
Key words: undecatungstozincoaluminic acid heteropol y acid catalyst