Synthesis and physicochemical characteristics of polymolybdenum(VI) phenylsiloxanes by means of different methods

Шапкин, Н. П.; Капустина, А. А.; Dombai, N. V.; Libanov, V. V.; Khal’chenko, I. G.; Gardionov, S. V.; Gribova, V. V.

doi:10.1007/s00289-019-02790-3

Cited by 6 publications

(6 citation statements)

References 14 publications

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“…Intense bands were also observed at 1134, 1029, 999 cm -1 , corresponding to stretching vibrations of ≡Si-Ph, ≡Si-O-Si≡ bonds, respectively; absorption bands at 495, 455 and 447 cm -1 correspond to deformation vibrations of bonds Si-O and Ca-O, respectively. Such a set of absorption bands corresponds to the vibrations of bond groups found in typical polymetalorganylsiloxanes [10].…”

Section: Resultsmentioning

confidence: 93%

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Synthesis of polycalciumphenylsiloxane and composites based on the skeleton of a sea urchin with the resulting polymer

et al. 2022

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In this work, we obtained polycalciumphenylsiloxane (PCPS) by the interaction of calcium bis (acetylacetonate) with polyphenylsiloxane. The first method consisted in boiling the starting reagents in toluene for several hours; the second was as follows: the mixture of the starting reagents was preliminarily treated mechanically in a ball mill, followed by boiling in toluene for several hours. Two fractions, soluble and insoluble, were isolated in both syntheses. They were investigated using IR, NMR spectroscopy, thermogravimetric analysis, and gel permeation chromatography. It was shown that the insoluble fraction is a mixture of calcium acetylacetonate and polyphenylsiloxane with a small calcium ion content. The soluble fraction is polycalciumphenylsiloxane. The yield of the soluble fraction is higher in the second synthesis method. The polymers obtained in the first and second synthesis methods are similar in composition and structure, which was confirmed by physicochemical methods. Next, the skeleton of the sea urchin Strongylocentrotus intermedius was treated with a soluble fraction in toluene. In this case, a composite was obtained, which was treated with 2–3% hydrochloric acid and then calcined at a temperature of 600 °C. At each stage, the composition of the composites was investigated using elemental analysis and IR spectroscopy. The morphology was investigated using scanning electron microscopy.

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Section: Resultsmentioning

confidence: 93%

“…The interaction of calcium bis (acetylacetonate) with polyphenylsiloxane was carried out in two different ways. Method 2 differed from method 1 by the use, in addition to boiling in toluene, of the preliminary mechanochemical treatment [10].…”

Section: Resultsmentioning

confidence: 99%

Synthesis of polycalciumphenylsiloxane and composites based on the skeleton of a sea urchin with the resulting polymer

et al. 2022

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“…The synthesis of PPhS was carried out using the method described in [ 50 ]. The data of the elemental analysis are given in Table 1 .…”

Section: Methodsmentioning

confidence: 99%

Silica-Containing Biomimetic Composites Based on Sea Urchin Skeleton and Polycalcium Organyl Silsesquioxane

Shapkin,

Khalchenko,

Drozdov

et al. 2023

Biomimetics

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The paper presents an original approach to the synthesis of polycalciumorganyl silsesquioxanes through the reaction of polyorganyl silsesquioxanes [RSiO1.5]n (where R is an ethyl and phenyl radical) with sea urchin skeleton under the conditions of mechanochemical activation. The novelty and practical significance of the present study lies in the use of an available natural raw source as a source of calcium ions to initiate the reaction of calcium silicate formation and create a matrix for the formation of a porous inorganic composite framework. The thermal stability of the introduced silicates, i.e., the ability to maintain a porous structure at high temperatures, is key to the production of an ordered porous material. The reaction scheme was proposed to be based on the interaction of calcium carbonate with the siloxane bond. FTIR, XRD, GPC, and TGA were used to study the composition and structure of the obtained materials. The cross-sectional area of the polymer chain and the volumes of the coherent scattering regions of the polymers obtained were calculated from the XRD data. To prepare the composites, the sea urchin skeleton was further modified with polycalciumorganyl silsesquioxanes in a toluene solution. To remove the sea urchin skeleton, the obtained biomimetic composites were treated with hydrochloric acid. The results of the morphological and surface composition studies are reported. The method proposed in the paper could be of fundamental importance for the possibility of obtaining structured porous composite materials for a wide range of practical applications, including for the purpose of creating a composite that may be a promising carrier for targeted delivery of chemotherapy agents.

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“…The method of mechanochemical activation is becoming more and more popular not only in the synthesis of inorganic and organic compounds [1][2][3][4][5][6][7][8], but also in the modi cation of elementorganic polymers [9][10][11][12][13][14]. It is widely used as one of the methods for modifying high molecular weight compounds, as well as for processing secondary polyole ns [15], removing persistent organic pollutants [16].…”

Section: Introductionmentioning

confidence: 99%

Interaction of Polyphenylsilsesquioxane With Various β-diketonate Complexes of Titanium By Mechanochemical Activation

Libanov

Капустина²,

Шапкин³

et al. 2022

Preprint

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In the present work, we studied the interaction of polyphenylsilsesquioxane with various β-diketonate complexes of titanium by mechanochemical activation. Polyphenylsilsesquioxane, bis-(2,4-pentanedionate) titanium dichloride, bis-(1-phenyl-1,3-butanedionate) titanium dichloride and bis-(1,3-diphenyl-1,3-propanedionate) titanium dichloride were used as starting reagents. Synthesis products were studied by various chemical and physicochemical methods of analysis. The composition of the obtained compounds has been determined. It is shown that under conditions of mechanochemical activation, high molecular weight products with a Si/Ti ratio different from the specified ones are formed. In addition, under the action of mechanical stresses, the initial titanium complexes (with the exception of acetylacetonate) polymerize with the formation of coordination high-molecular compounds, which are destroyed by the addition of ethyl alcohol. The work is fundamental and contributes to the understanding of the mechanisms of mechanochemical synthesis. The work is aimed at finding effective and environmentally friendly methods for the synthesis and modification of elementorganic high-molecular compounds.

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Synthesis and physicochemical characteristics of polymolybdenum(VI) phenylsiloxanes by means of different methods

Cited by 6 publications

References 14 publications

Synthesis of polycalciumphenylsiloxane and composites based on the skeleton of a sea urchin with the resulting polymer

Synthesis of polycalciumphenylsiloxane and composites based on the skeleton of a sea urchin with the resulting polymer

Silica-Containing Biomimetic Composites Based on Sea Urchin Skeleton and Polycalcium Organyl Silsesquioxane

Interaction of Polyphenylsilsesquioxane With Various β-diketonate Complexes of Titanium By Mechanochemical Activation

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