(1 遼寧大學(xué)化學(xué)科學(xué)與工程學(xué)院,沈陽 110036;
2 東北大學(xué)材料與冶金學(xué)院, 沈陽 110006)
摘 要: 采用離子交換.冷凍法制得11-鎢鋅合鋁雜多酸[H7HAl(H2O)ZnW11O39]·12H2O。確定了反應(yīng)的pH值和物料的最佳比。 用元素分析、電位滴定、紅外光譜、紫外光譜、X射線粉末衍射和熱分析等對(duì)合成產(chǎn)物進(jìn)行了表征。電位滴定表明其7個(gè)質(zhì)子是兩步離解的。 紅外光譜給出了4個(gè)特征峰, 紫外光譜給出了兩個(gè)強(qiáng)的荷移躍遷譜帶。根據(jù)X射線粉末衍射實(shí)驗(yàn)結(jié)果, 確認(rèn)11-鎢鋅合鋁雜多酸具有Keggin結(jié)構(gòu)。 在此基礎(chǔ)上,對(duì)其在合成己二酸二(2-乙基己)酯(DOA)中的催化性能進(jìn)行了研究,其選擇性為99.9%,產(chǎn)率為93.9%。
關(guān)鍵字: 11-鎢鋅合鋁酸 雜多酸 催化劑
(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


