碱和碱土钼酸盐的快速高效机械合成†。

Andres Lara-Contreras, Patrick Julien, Jennifer Scott and Emily C. Corcoran
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摘要

复杂钼酸盐的传统制备方法是固态合成法和水化学法,这些方法通常需要较长的反应时间和较大的溶剂用量或较高的烧结温度。然而,这些技术通常会产生不想要的次生物质、不完全反应和相对较低的产率。事实证明,机械化学法对合成复杂的钼酸盐非常有效。这项工作进一步发展了各种七钼酸盐(即钠、铷和铯)和三钼酸盐(即钠、铷、铯、锶和钡)的机械化学合成。获得的材料通过粉末 X 射线衍射、傅立叶变换红外光谱、拉曼光谱、热重分析和扫描电子显微镜进行表征,以评估样品的纯度、形态和质量。在不到三小时的反应时间内,就获得了各种三钼酸盐和七钼酸盐的高纯度样品,且能量输入和副产品极少。机械化学为合成各种三钼酸盐和七钼酸盐(包括三钼酸钠的一水合物形式,而不是通常从水溶液反应中获得的三水合物变体)提供了一种快速、更可持续且简单的程序。
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Rapid and efficient mechanosynthesis of alkali and alkaline earth molybdates†

Complex molybdates are traditionally prepared via solid-state synthesis and aqueous chemistry methods, which generally require long reaction times and large solvent volumes or high sintering temperatures. However, these techniques often result in undesired secondary species, incomplete reactions, and relatively low yields. Mechanochemistry has proven effective for the synthesis of complex molybdates. This work expands on the development of the mechanochemical synthesis of various heptamolybdates (i.e., sodium, rubidium, and cesium), and trimolybdates (i.e., sodium, rubidium, cesium, strontium, and barium). The obtained materials were characterized via powder X-ray diffraction, Fourier-transform infrared spectroscopy, Raman spectroscopy, thermo-gravimetric analysis, and scanning electron microscopy to assess the purity, morphology, and quality of the sample. High purity samples of the various trimolybdates and heptamolybdates were obtained in less than three hours of reaction time, with minimal energy input and by-products. Mechanochemistry provides a fast, more sustainable, and simple procedure for the synthesis of a wide variety of both trimolybdates and heptamolybdates including the monohydrate form of sodium trimolybdate instead of the trihydrate variant commonly obtained from aqueous reactions.

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Back cover Moving mechanochemistry forward Influence of ball milling parameters on the mechano-chemical conversion of polyolefins. Mechanochemical synthesis of rock salt-type Na2CaSnS4 as a sodium-ion conductor† Mechanochemical synthesis and transformation of the polymorphic double carbonates fairchildite and buetschliite, (K2Ca(CO3)2): an in situ X-ray powder diffraction study†
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