A kind of preparation method of high nuclear metal manganese cluster

Abstract

The invention provides a method for preparing a polyanion Na8H32[{MnIV24MnIII12O28(H2O)23}2(W24O120)2]*66H2O (marked as Mn72W48). The method comprises the following steps: dissolving Mn(CH3COO)2 and KMnO4 into a diluted CH3COOH solution, conducting continuous stirring so as to obtain a sol.Mn solution, gradually adding a Na2WO4 solution into the sol.Mn solution, increasing the pH value of the sol.Mn solution to about 5.5 through the alkalinity of Na2WO4, so as to obtain a sol.Mn-W solution, conducting heating, cooling and filtering on the sol.Mn-W solution, and conducting evaporation, so as toobtain the polyanion. By adopting the synthesis process provided by the invention, the concentration of a manganese substance in the solutions is greatly increased, mass spectrum signals of a low-nucleus manganese cluster in the solutions have no monitoring blind areas, and the synthesis quality and efficiency are greatly improved.

Description

technical field [0001] The invention belongs to the field of preparation of high-nuclear metal manganese clusters, in particular to a polyanion Mn 72 W 48 method of preparation. Background technique [0002] High-nuclear manganese clusters have great application value in the fields of catalysis, magnetism, and medicine, and thus have received extensive attention. The method of synthesizing high-nuclear manganese clusters is usually to use organic ligands to connect low-nuclear manganese clusters, but the disadvantage of this method is that it needs to use toxic, volatile and highly flammable organic solvents. Polyoxometalates (POMs), as inorganic multidentate ligands, have the characteristics of variable and controllable structures, and can be reacted in the aqueous phase to synthesize high-nuclear metal clusters, thus making the whole reaction more economical and environmentally friendly. However, polyoxometalates (POMs) are clustered as inorganic multi-dentate ligands, ...

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Problems solved by technology

It can be known by calculation that after the reaction raw materials are uniformly mixed, the ratio of the amount of tungstate and Mn species is about 45:1 (there is 1g sodium tungstate and 0.045g Mn in the solution 12 ), the high-resolution mass spectrometry signals of manganese species are mostly covered by the high concentration of tungstate and cannot be detected, which limits the monitoring of the synthesis process of this compound and restricts the detection of other low-nuclear manganese clusters that exist in the synthesis process. change research

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