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上岸1112

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[求助] UIO66-(COOH)2个合成方法求助或者问题解答 已有1人参与

本人目前在合成UIO66-(COOH)2,但是扫描拍不到参考文献中那种规则的形貌,合成方法试过好几种,目前还没有找到正确的方法

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ca0yan9

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【答案】应助回帖

文献给出的合成方法:
UiO-66的固体样品通常是经过经典的溶剂热方法晶化而得,将锆源ZrCl4与配体H2BDC溶解在溶剂DMF中,形成晶化母液,在120 ℃下静态晶化24 h,经过洗涤与干燥后即可得到晶体尺寸约为150 nm,形貌近似为立方的UiO-66固体样品。(高稳定性金属有机骨架UiO-66的合成与应用, Chinese Journal of Applied Chemistry, 33(4): 367-378)
UiO-66-(COOH)2合成:A mixture of ZrO(NO3)2·xH2O (100 mg, 0.43 mmol),H2BDC-CO2H (182 mg, 0.86 mmol) and benzoic acid (1.58 g,12.94 mmol) in 3 mL of N,N’-dimethyformamide (DMF) was 85 placed in a glass tube (10 mL). The tube was sealed and heated in a programmable heating block to 150 ºC at a rate of 2.2 ºC min-1, held at this temperature for 24 h, then cooled to room temperature at a rate of 2.2 ºC min-1. (10.1039/C3DT32288B)
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