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Mechanochemical Synthesis of Ca- and Mg-Double Salt Crystalline Materials Using Insoluble Alkaline Earth Metal Bearing Minerals

机译:使用不溶性碱土金属轴承矿物的Ca-和Mg双盐晶材料的机械化学合成

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摘要

Sustainable, liquid-assisted grinding mechanochemical synthesis of crucial nutrient containing compounds, namely, Ca-and Mg-struvites (CaNH4PO4 center dot H2O and MgNH4PO4 center dot 6H(2)O) and complex double salts (Ca(NH4)(2)(HPO4)(2)center dot H2O dimorph B, Mg(NH4)(2)(HPO4)(2)center dot 4H(2)O dimorph A), was performed. These compounds were synthesized using solid crystalline monoammonium phosphate (NH4H2PO4, MAP) and low solubility common calcium and magnesium minerals, such as hydroxides, carbonates, and oxides. Powder X-ray diffraction showed single crystalline phase materials. Properties of the synthesized compounds were studied by thermogravimetric analysis/ differential scanning calorimetry (TGA/DSC), Raman spectroscopy, and dynamic vapor sorption (DVS). TGA results showed that Ca-struvite was the most thermally robust, followed by Ca- and Mg-complex double salts and Mg-struvite. The decomposition of samples with release of NH3 was marked by peaks in the DSC profiles at 190 degrees C for both complex double salts and a broad DSC shoulder at 186 degrees C was observed for struvites. Raman spectroscopy showed the presence of distorted PO43- bands due to protonation of the phosphate species and multiple binding environments. DVS measurements showed that these compounds deliquesced at very high relative humidity conditions (similar to 90%), which in some cases led to significant changes in the dominant crystalline phase.
机译:可持续,液体辅助研磨机械化学合成关键营养化合物,即Ca-and Mg-struvites(CanH 4PO4中心点H2O和MgNH4PO4中心点6H(2)O)和复合双盐(Ca(NH4)(2)( HPO4)(2)中央点H2O二聚体B,Mg(NH4)(2)(2)(2)中心点4H(2)O二聚体A)。这些化合物使用固体结晶磷酸酯(NH 4 H 2 PO 4,MAP)和低溶解度普通钙和镁矿物,例如氢氧化物,碳酸盐和氧化物合成。粉末X射线衍射显示单晶相材料。通过热重分析/差示扫描量热法(TGA / DSC),拉曼光谱和动态蒸汽吸附(DVS)研究了合成化合物的性质。 TGA结果表明,Ca-Struvite是最热稳健的,其次是Ca-和Mg-复杂的双盐和Mg-斯特氏。对于释放NH 3的样品的分解,在190摄氏度下,在190摄氏度下,对于斯特鲁维特观察到两个复合双盐和186摄氏度的宽DSC肩部。拉曼光谱表现出由于磷酸盐物质的质子化和多个结合环境而存在扭曲的PO43-带。 DVS测量表明,这些化合物在非常高的相对湿度条件下(类似于90%),在某些情况下,在某些情况下导致了显性结晶相的显着变化。

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