In the present work, polyaluminophenylsiloxanes have been obtained by two methods: the first one consisted in the exchange of sodium phenylsilanolate with aluminum chloride in an anhydrous medium (dimethyl sulfoxide-toluene), while the second one—in the reaction of aluminum acetylacetonate with polyphenylsiloxane under the conditions of mechanochemical activation. The polymers were purified by re-precipitation in the first case and by toluene extraction in the second case. The obtained aluminophenylsiloxanes have been studied by the methods of gel chromatography, diffractometry, and IR and 13C, 29Si, and 27Al NMR spectroscopy. It has been shown that the interaction under the conditions of mechanochemical activation proceeded in two directions: the Si–O–Si bond splitting reaction and the condensation reaction. A comparison of the physical and chemical characteristics of polyaluminophenylsiloxanes has been carried out, and it has been demonstrated that the structure of the PAlPhSi is structurally more homogeneous; aluminophenylsiloxy fragments were present along with siloxyaluminoacetylacetone fragments in PAl(acac)PhSi, which significantly complicated the polymer structure. © 2021, The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.

Ссылка на оригинал статьи