Transactions of Nonferrous Metals Society of China The Chinese Journal of Nonferrous Metals

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中国有色金属学报

ZHONGGUO YOUSEJINSHU XUEBAO

第8卷    第2期    总第27期    1998年6月

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文章编号:(1998)02-327-4
11-钨锌合铝杂多酸的合成和表征及其催化性能
吴庆银1,2    翟玉春2

(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

SYNTHESIS, CHARACTERIZATION AND CATALYTIC PERFORMANCE OF UNDECATUNGSTOZINCOALUMINIC HETEROPOLY ACID
Wu Qingyin1,2 and Zhai Yuchun2

(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

ISSN 1004-0609
CN 43-1238/TG
CODEN: ZYJXFK

ISSN 1003-6326
CN 43-1239/TG
CODEN: TNMCEW

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