Coordination Compounds of Cobalt(II) Nitrate and Perchlorate with Acetamide and Carbamide: Precursors for the Synthesis of Catalytically Active Tricobalt Tetraoxide

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Abstract

The reactions of cobalt(II) nitrate or perchloride with acetamide (AA) or carbamide (Ur) in an aqueous medium produce coordination compounds [Co(Ur)4](NO3)2 (I), [Co(Ur)6](NO3)2 (II), [Co(AA)4(H2O)2](NO3)2 (III), [Co(AA)4(H2O)2](NO3)2 ∙ 2AA (IV), [Co(Ur)6](ClO4)2, (V), [Co(AA)4(H2O)2](ClO4)2 (VI), and [Co(AA)6](ClO4)2 (VII). The compositions of the isolated complexes are determined by physicochemical methods, and the crystal and molecular structures of compounds II, V, VI, and VII are solved. Specific features of the thermal behavior of all synthesized compounds in a wide temperature range are studied in detail. These compounds are shown to be used as precursors in the preparation of nanosized Co3O4 using self-propagating high-temperature synthesis. The catalytic activity of thus synthesized Co3O4 in the model epoxidation of allyl alcohol is studied.

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R. A. Rodriguez Pineda

MIREA Russian Technological University

Author for correspondence.
Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

I. A. Karavaev

MIREA Russian Technological University

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

E. V. Savinkina

MIREA Russian Technological University

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

E. V. Volchkova

MIREA Russian Technological University

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

Zh. Yu. Pastukhova

MIREA Russian Technological University

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

L. G. Bruk

MIREA Russian Technological University

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

G. A. Buzanov

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

A. S. Kubasov

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

V. M. Retivov

Kurchatov Institute

Email: rodrigues.pineda@yandex.ru
Russian Federation, Moscow

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Supplementary files

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2. Scheme 1

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3. Fig. 1. Diffractograms of starting substances and isolated nitrate complexes: 1 - urea, 2 - acetamide, 3 - Co(NO3)2 . 6H2O, 4 - I (exp.), 5 - II (exp.), 6 - II (calculated), 7 - III (exp.), 8 - IV (exp.)

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4. Fig. 2. Diffractograms of initial substances and isolated perchlorate complexes: 1 - Co(ClO4)2 . . 6H2O, 2 - V (exp.), 3 - V (calculated), 4 - VI (exp.), 5 - VI (calculated), 6 - VII (exp.), 7 - VII (calculated)

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5. Fig. 3. Fragment of structure II

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6. Fig. 4. Fragment of the structure V

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7. Fig. 5. Fragment of structure VI

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8. Fig. 6. Fragment of structure VII

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9. Fig. 7. Thermogram of the complex [Co(Ur)4](NO3)2 (I)

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10. Fig. 8. Thermogram of the complex [Co(AA)4(H2O)2](ClO4)2 (VI)

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11. Fig. 9. Diffractogram of the solid product of thermolysis of complex V (* denotes reflections characteristic of Co3O4)

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12. Fig. 10. Microphotographs of the thermolysis product of samples I (a), II (b) and V (c)

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13. Fig. 11. Particle size distribution of Co3O4 obtained by thermolysis of compounds I, II and V

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