Studies of Interaction of Polyphenylsiloxane with Vanadyl Bis-Acetylacetonate

Шапкин, Н. П.; Капустина, А. А.; Gardionov, S. V.; Khal’chenko, I. G.; Libanov, V. V.; Tokar, Eduard

doi:10.1007/s12633-017-9551-z

Cited by 7 publications

(8 citation statements)

References 5 publications

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“…Earlier in [12] it was shown that heating the products of the interaction of vanadium bis (acetylacetonate) with polyphenylsiloxane to 300 °C sharply increased the yield of the target product due to the removal of acetylacetonate groups and the formation of the -M-O-Si≡ bond. The TG-DTA curve of insoluble fraction 1.2 (Figure 6) shows three exothermic effects at 290, 380, and 460 °C, the weight loss at which is 43%, while the mass of acetylacetonate groups in the gross formula (Table 1) corresponds to 40%.…”

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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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: 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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“…2.8 Nuclear magnetic resonance. NMR spectra were recorded on an Avance 400 MHz high-resolution spectrometer (Bruker, Germany) on 1 H and 13 C nuclei at different operating frequencies. Deuterated chloroform and dimethyl sulfoxide-d 6 were used as solvents.…”

Section: Interaction Of Polyphenylsilsesquioxane With Dichlorobis-(3-oxo-13-diphenylprop-1-en-1-olate) Titanium (Iv)mentioning

confidence: 99%

“…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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“…Here, it was shown that the silicon-oxygen-boron bond was disrupted with an increase of the activation time and the weight of the grinding balls. Several studies have been conducted on the interaction of metal acetylacetonates with polyphenylsiloxane under the conditions of mechanochemical activation [15][16][17][18].…”

Section: Introductionmentioning

confidence: 99%

“…Analyzing the obtained data on the synthesis of polymetallosiloxanes under mechanochemical activation, one should mention that the interaction of polyorganylsiloxane with metal acetylacetonate proceeded in depth for elements that formed acidic oxides, for example, boron [17], phosphorus [19], and compounds of amphoteric elements [12,13]. In case of d-metal complexes, the reaction proceeded with difficulty [11,16,18] and at an increased temperature [18]. In particular, a temperature increase up to 300°C after mechanochemical activation resulted in a significant increase of the yield of vanadium-containing phenylsiloxane and an attaining to the initial ratio of silicon to vanadium [16].…”

Section: Introductionmentioning

confidence: 99%

Fabrication of Magnesium-Silicon Nanocomplexes by the Interaction of Polyphenylsiloxane with Magnesium Carbonate

Шапкин

Maslova

Papynov

et al. 2021

MSF

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The interaction of magnesium carbonate with polyphenylsiloxane under the conditions of mechanochemical activation with subsequent heating has been investigated. Based on the TGA and DTA data, it has been shown that, upon heating up to 420°C, the reaction proceeded completely with the release of carbon dioxide. The polymer was dissolved in DMFA and purified by repeated precipitation with water. The polymer yield was 64%. The residue insoluble in organic solvents has been obtained by evaporation of an aqueous solution. The composition and structure of the synthesis products have been analyzed by means of element analysis, IR spectroscopy, and diffractometry. It has been demonstrated that the fraction soluble in DMFA had a silicon-to-magnesium ratio equal to 4.2, while the fraction isolated from water had this ratio equal to 1.0. The IR and XRD data enabled one to conclude that, regardless of the different compositions, the structures of all fractions were similar and corresponded to mesomorphic layered polymers produced by the ion exchange method.

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Studies of Interaction of Polyphenylsiloxane with Vanadyl Bis-Acetylacetonate

Cited by 7 publications

References 5 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

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

Fabrication of Magnesium-Silicon Nanocomplexes by the Interaction of Polyphenylsiloxane with Magnesium Carbonate

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