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本文以气相色谱为主要手段,配合红外光谱、X—射线粉末衍射分析及电子顺磁共振技术,研究了十二钼磷酸及其盐在氢气中的还原热稳定性。从对上述化合物在氢气中热解过程的气相产物和各中间固相产物的分析可知,在实验的温度范围内(40～640℃),这些化合物的热分解过程通常分为三或四个阶段。实验发现,Keggin阴离子热解以及Mo~(6+)被还原的难易程度,取决于与Keggin阴离子结合的阳离子的种类。在同一实验条件下,如果阳离子本身难以还原,那么,Keggin阴离子的破坏以及Keggin阴离子中Mo~(6+)还原为金属相的过程,都将变得困难。
In this paper, gas chromatography as the main means, combined with infrared spectroscopy, X-ray powder diffraction and electron paramagnetic resonance technology, the dodecamethylene phosphonic acid and its salts in the reduction of hydrogen thermal stability. From the analysis of the gas phase products and intermediate solid products of pyrolysis of the above compounds in hydrogen, it can be seen that the thermal decomposition of these compounds is generally divided into three or four stages within the experimental temperature range (40-640 ° C) . It was found that the pyrolysis of Keggin anion and the ease of reduction of Mo ~ (6+) depend on the type of cations bound to Keggin anion. Under the same experimental conditions, if the cation itself is hard to be reduced, the destruction of Keggin anion and the reduction of Mo ~ (6+) in the Keggin anion to the metal phase will be difficult.