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Study of the Reaction Products of TaCl5 with Acetylene in Benzene–a Catalyst for Alkyne Cyclotrimerization

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Abstract—

Products of reaction between TaCl5 and C2H2 in benzene, with the composition TaCl3.7C15H22—heterogeneous catalysts for cyclotrimerization of alkynes—have been studied using scanning electron microscopy, IR spectroscopy, and X-ray photoelectron spectroscopy (XPS). The catalysts consist of spherical particles with an average diameter of 70 nm. According to the XPS results, the elemental composition of their surface is TaCl1.80C28O3. The tantalum 4f7/2 and 5p3/2 binding energies (Eb) obtained, 26.3 and 37.2 eV, indicate that the oxidation state of tantalum on the surface of the material is 5+. After Ar+ ion etching, we observe, in addition to Ta5+, 4f7/2 and 5p3/2 lines at Eb = 23.8 and 34.6 eV, respectively, which demonstrates that the oxidation state of tantalum in the active catalyst is 3+. The Cl 2p line has the form of two overlapping doublets with binding energies of 198.7 and 200.1 eV, due to the presence of bridging and terminal chlorine atoms in the catalytically active complex. The binding energy Eb(C 1s) = 284.2 eV corresponds to cyclic unsaturated hydrocarbons with conjugated bonds of the hydrocarbon matrix. The catalyst is stable in high vacuum and undergoes no charging when exposed to an X-ray beam, which suggests that it has weak dielectric properties.

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Funding

This work was supported through the state research target for the Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, project no. 01201353365.

We acknowledge the support from the Russian Federation Ministry of Science and Higher Education.

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Authors and Affiliations

  1. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, 119991, Moscow, Russia

    E. G. Il’in, A. S. Parshakov & V. G. Yarzhemsky

  2. Kurchatov Institute National Research Centre, 123182, Moscow, Russia

    A. Yu. Teterin & Yu. A. Teterin

  3. Moscow State University, 119991, Moscow, Russia

    K. I. Maslakov & Yu. A. Teterin

Authors
  1. E. G. Il’in
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  2. A. S. Parshakov
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  3. A. Yu. Teterin
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  4. K. I. Maslakov
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  5. V. G. Yarzhemsky
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  6. Yu. A. Teterin
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Correspondence to E. G. Il’in.

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Il’in, E.G., Parshakov, A.S., Teterin, A.Y. et al. Study of the Reaction Products of TaCl5 with Acetylene in Benzene–a Catalyst for Alkyne Cyclotrimerization. Inorg Mater 58, 845–853 (2022). https://doi.org/10.1134/S0020168522070093

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  • DOI: https://doi.org/10.1134/S0020168522070093

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