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Insights into the Mechanochemical Synthesis of MOF-74

机译：洞察MOF-74的机械化学合成

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摘要

Mechanochemical synthesis has recently emerged as a scalable "green" approach for the preparation of MOFs, but current understanding of the underlying reaction mechanisms is limited. In this work, an investigation of the reaction pathway of the mechanochemical synthesis of MOF-74 from ZnO and 2,5-dihydroxyterephthalic acid (H(4)HDTA), using DMF as a liquid additive, is presented. The complex reaction pathway involves the formation of four short-lived intermediate phases, prior to the crystallization of MOF-74. The crystal structures of three of these intermediates have been determined using a combination of single-crystal and powder X-ray diffraction methods and are described here. The initial stages of the reaction are very fast, with a DMF solvate of H(4)HDTA forming after only 2 min of milling. This is followed by crystallization, after only 4 min of milling, of a triclinic one-dimensional coordination polymer, Zn(H(2)DHTA)(DMF)(2)(H2O)(2), which converts into a monoclinic polymorph on additional milling. Highly crystalline MOF-74 appears after prolonged milling, for at least 70 min.
机译：机械力化学合成最近成为一种可扩展的“绿色”MOF制备方法，但目前对潜在反应机制的理解有限。本文研究了以氧化锌和2,5-二羟基对苯二甲酸（H（4）HDTA）为原料，DMF为液体添加剂，机械力化学合成MOF-74的反应途径。复杂的反应途径包括在MOF-74结晶之前形成四个短寿命的中间相。其中三种中间体的晶体结构已使用单晶和粉末X射线衍射法相结合的方法确定，本文对此进行了描述。反应的初始阶段非常快，仅在研磨2分钟后形成H（4）HDTA的DMF溶剂化物。随后，在仅研磨4分钟后，三斜一维配位聚合物Zn（H（2）DHTA）（DMF）（2）（H2O）（2）结晶，其在额外研磨时转化为单斜多晶型。在长时间研磨至少70分钟后，会出现高度结晶的MOF-74。

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