The formation of polymeric acetylacetonates of magnesium, aluminum, iron, zirconium, and vanadyl under conditions of mechanochemical activation with subsequent condensation in boiling toluene has been investigated. The obtained compounds have been studied by the methods of gel chromatography, X-ray diffractometry, and positron annihilation and IR spectroscopy. Aluminum chelates have been studied by means of NMR spectroscopy. It has been demonstrated that the mechanochemical activation with subsequent boiling in toluene results in the formation of polymeric chelates, mostly those of iron, zirconium and, to a smaller degree, chelates of aluminum, magnesium, and vanadyl. The molecular weight of soluble high-molecular fractions is in the range 3000–5000 Da. The layered polymer structure has been revealed. Cross-section areas of polymer chains and volumes of coherent scattering regions have been calculated from the diffractometry data. The morphology of polymers consisting of spherical particles of sizes in the range 100–700 nm has been investigated. Based on the data of positron annihilation spectroscopy (PAS), density, and nitrogen low-temperature adsorption, the dependence of the chelate stability on the specific polarizing potential has been determined. A fractal structure of solid-state polychelates has been revealed. © 2021 Trans Tech Publications Ltd, Switzerland.

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