In Situ and Ex Situ Studies of Tetrammineplatinum(II) Chromate Thermolysis

Lagunova, Varvara; Filatov, E. Yu.; Plyusnin, P. E.; Korenev, S. V.

doi:10.1134/s0036023620100150

Cited by 11 publications

(3 citation statements)

References 23 publications

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“…Another typical study of the catalyst synthesis by means of in situ XRD includes the decomposition of precursor, such as formation of nickel oxide from Ni 3 (NO 3 ) 2 (OH) 4 [92], copper oxide from copper nitrate [93]; transformation of CeCO 3 OH to CeO 2 [94]; decomposition of Ce and Mn oxalates to mixed Mn-Ce oxides [95]; preparation of WOx-CeO 2 catalysts [96]; formation of Pd-containing zirconia oxide from amorphous precursor [97]; thermolysis of [Pt(NH 3 ) 4 ]CrO 4 complex [98], preparation porous mixed-valent manganese oxides by hydrothermal treatment of layered precursor [99], by thermal decomposition of KMnO 4 [100].…”

Section: Study Of the Preparation Proceduresmentioning

confidence: 99%

In Situ X-ray Diffraction as a Basic Tool to Study Oxide and Metal Oxide Catalysts

Bulavchenko,

Vinokurov

2023

Catalysts

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X-ray diffraction (XRD) is a standard technique that is widely applied in heterogeneous catalysis to determine phase composition, atomic structure, and size of crystallites. This review is focused on the application of in situ XRD for studying the catalysts during their “lifetime” (under synthesis, activation, operation, and deactivation conditions), limiting the objects of research to oxide and metal oxide catalysts. Also included is a brief overview of modern techniques and instruments and the latest works illustrating different aspects of this technique in catalyst research. The main conclusion is that the field of heterogeneous catalysis research would benefit substantially from the application of in situ XRD for the structural, phase, and morphological characterization of solid catalysts. Even more useful information can be obtained if XRD is combined with other techniques that are more sensitive at length scales different from that of XRD.

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Section: Study Of the Preparation Proceduresmentioning

confidence: 99%

In Situ X-ray Diffraction as a Basic Tool to Study Oxide and Metal Oxide Catalysts

Bulavchenko,

Vinokurov

2023

Catalysts

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“…An easy and convenient reaction route for the preparation of the simple and mixed nanosized transition metal oxides [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18]-especially for the synthesis of catalytically active spinel oxides [19][20][21][22][23][24][25][26][27][28][29][30]-is the thermal decomposition of complexes having reducing ligands and oxidizing anions [31][32][33][34][35][36][37][38]. These processes consisted of a solid-phase quasiintramolecular redox reaction between an oxidizing anion and a reducing ligand.…”

Section: Introductionmentioning

confidence: 99%

Insight into the Structure and Redox Chemistry of [Carbonatotetraamminecobalt(III)] Permanganate and Its Monohydrate as Co-Mn-Oxide Catalyst Precursors of the Fischer-Tropsch Synthesis

Béres,

Dürvanger,

Homonnay

et al. 2024

Inorganics

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[Carbonatotetraamminecobalt(III)] permanganate monohydrate was synthesized first in the metathesis reaction of [Co(NH3)4CO3]NO3 and NaMnO4 in aqueous solution. Its thermal dehydration at 100 °C resulted in phase-pure [Co(NH3)4CO3]MnO4 (compound 1). Compounds 1 and 2 (i.e., the hydrated form) were studied with IR, far-IR, and low-temperature Raman spectroscopies, and their vibrational modes were assigned. The lattice parameters were determined by powder X-ray diffraction (PXRD) and single crystal X-ray diffraction (SXRD) methods for the triclinic and orthorhombic compounds 1 and 2, respectively. The detailed structure of compound 2 was determined, and the role of hydrogen bonds in the structural motifs was clarified. UV studies on compounds 1 and 2 showed the distortion of the octahedral geometry of the complex cation during dehydration because of the partial loss of the hydrogen bonds between the crystal water and the ligands of the complex cation. The thermal decomposition consists of a solid phase quasi-intramolecular redox reaction between the ammonia ligands and permanganate anions with the formation of ammonia oxidation products (H2O, NO, N2O, and CO2). The solid phase reaction product is amorphous cobalt manganese oxide containing ammonium, carbonate (and nitrate) anions. The temperature-controlled thermal decomposition of compound 2 in toluene at 110 °C showed that one of the decomposition intermediates is ammonium nitrate. The decomposition intermediates are transformed into Co1.5Mn1.5O4 spinel with MnCo2O4 structure upon further heating. Solid compound 2 gave the spinel at 500 °C both in an inert and air atmosphere, whereas the sample pre-treated in toluene at 110 °C without and with the removal of ammonium nitrate by aqueous washing, gave the spinel already at 300 and 400 °C, respectively. The molten NH4NO3 is a medium to start spinel crystallization, but its decomposition stops further crystal growth of the spinel phase. By this procedure, the particle size of the spinel product as low as ~4.0 nm could be achieved for the treatments at 300 and 400 °C, and it increased only to 5.7 nm at 500 °C. The nano-sized mixed cobalt manganese oxides are potential candidates as Fischer-Tropsch catalysts.

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“…The temperature-controlled decomposition of transition metal complexes containing redox-active central atoms, ligands, and anions in solid-phase quasi-intramolecular redox reactions has become a widely used method of preparing nano-sized oxides, nitrides, carbides, metals, and their alloys [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19]. The reducing ligands (pyridine, urea, or ammonia) and oxidizing anions containing precursors frequently give amorphous decomposition intermediates, which can be transformed into controlled-sized crystalline materials by heat treatment [7,[10][11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26][27][28].…”

Section: Introductionmentioning

confidence: 99%

Review on the Chemistry of [M(NH3)n](XO4)m (M = Transition Metal, X = Mn, Tc or Re, n = 1–6, m = 1–3) Ammine Complexes

Mehrotra

2023

Inorganics

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The preparation of ammine complexes of transition metals having oxidizing anions such as permanganate and perrhenate ions is a great challenge due to possible reactions between ammonia and oxidizing anions during the synthesis of these materials. However, it has an important role in both the development of new oxidants in organic chemistry and especially in the preparation of mixed-metal oxide catalyst precursors and metal alloys for their controlled temperature decomposition reactions. Therefore, in this paper, synthetic procedures to prepare ammonia complexes of transition metal permanganate, pertechnetate, and perrhenate (the VIIB group tetraoxometallates) salts have been comprehensively reviewed. The available data about these compounds’ structures and spectroscopic properties, including the presence of hydrogen bonds that act as redox reaction centers during thermal decomposition, are given and evaluated in detail. The nature of the thermal decomposition products has also been summarized. The available information about the role of the ammine complexes of transition metal permanganate salts in organic oxidation reactions, such as the oxidation of benzyl alcohols and regeneration of oxo-compounds from oximes and phenylhydrazones, including the kinetics of these processes, has also been collected. Their physical and chemical properties, including the thermal decomposition characteristics of known diammine (Ag(I), Cd, Zn, Cu(II), Ni(II)), triammine (Ag(I)), and simple or mixed ligand tetraammine (Cu(II), Zn, Cd, Ni(II), Co(II), Pt(II), Pd(II), Co(III)), Ru(III), pentaammine (Co(III), Cr(III), Rh(III) and Ir(III)), and hexaammine (Ni(II), Co(III), Cr(III)) complexes of transition metals with tetraoxometallate(VII) anions (M = Mn, Tc and Re), have been summarized. The preparation and properties of some special mixed ligand/anion/cation-containing complexes, such as [Ru(NH3)4(NO)(H2O)](ReO4)2, [Co(NH3)5(H2O)](ReO4)2, [Co(NH3)5X](MnO4)2 (X = Cl, Br), [Co(NH3)6]Cl2(MnO4), [Co(NH3)5ReO4]X2 (X = Cl, NO3, ClO4, ReO4), and K[Co(NH3)6]Cl2(MnO4)2, are also included.

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In Situ and Ex Situ Studies of Tetrammineplatinum(II) Chromate Thermolysis

Cited by 11 publications

References 23 publications

In Situ X-ray Diffraction as a Basic Tool to Study Oxide and Metal Oxide Catalysts

In Situ X-ray Diffraction as a Basic Tool to Study Oxide and Metal Oxide Catalysts

Insight into the Structure and Redox Chemistry of [Carbonatotetraamminecobalt(III)] Permanganate and Its Monohydrate as Co-Mn-Oxide Catalyst Precursors of the Fischer-Tropsch Synthesis

Review on the Chemistry of [M(NH3)n](XO4)m (M = Transition Metal, X = Mn, Tc or Re, n = 1–6, m = 1–3) Ammine Complexes

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