Preparation and characterization of benzotriazolium perrhenate

Louis–Jean, James; Jang, Harry; Lawler, Keith V.; Forster, Paul M.; Ash, Jeffrey; Poineau, Frédéric

doi:10.1016/j.ica.2019.119121

Cited by 3 publications

(7 citation statements)

References 42 publications

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“…The C 6 H 6 N 3 [ReO 4 ] salt crystallizes in the monoclinic space group P 2 1 / c ( a = 12.854(2) Å; b = 4.9121(8) Å; c = 14.819(2) Å) and its structure is stabilized by hydrogen bonds. , In BPR, tetrahedral [ReO 4 ] − anions are slightly distorted and neighboring anions exhibit van der Waals interaction, which form chains of ReO1···ReO1 along the crystallographic b -axis. White needlelike BPR is air-stable and can be stored for months without apparent decomposition.…”

Section: Resultsmentioning

confidence: 99%

“…White needlelike BPR is air-stable and can be stored for months without apparent decomposition. A recent analysis (experimental and theoretical) 16 indicated that the behavior of BPR in solution is governed by the nature of benzotriazole species (e. g., C 6 H 6 N 3 + , C 6 H 4 N 3 − ) and solvent pK a (Figure 1).…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…These chemicals were used as received without any further purification. The C 6 H 6 N 3 [ReO 4 ] salt was prepared following the method described in the literature , and characterized in solution (UV–visible spectroscopy) and in the solid state (powder X-ray diffraction; see Figure ) prior to this study. All mixed powdered samples were prepared by pulverizing (3×) solid Re material and BTA (C 6 H 5 N 3 ) using a mortar and pestle at room temperature.…”

Section: Methodsmentioning

confidence: 99%

“…These chemicals were used as received without any further purification. The C 6 H 6 N 3 [ReO 4 ] salt was prepared following the method described in the literature 16,17 and characterized in solution (UV−visible spectroscopy) and in the solid state (powder X-ray diffraction; see Figure 1) prior to this study. All…”

Section: ■ Conclusionmentioning

confidence: 99%

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Thermal Analysis of Benzotriazolium Perrhenate and Its Implication to Rhenium Metal

et al. 2021

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The thermal analysis behavior of C 6 H 6 N 3 [ReO 4 ] was studied by simultaneous thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) up to 700 °C under argon. Such analysis afforded rhenium metal, which was characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), and energy-dispersive X-ray (EDX) spectroscopy. XRD peak broadening due to crystallite size and lattice strain was analyzed by both Williamson−Hall (W−H) and Debye−Scherrer (D−S) methods. Efforts to isolate Re metal from the thermal treatment of benzotriazole (BTA = C 6 H 5 N 3 ) with NH 4 ReO 4 and Re 2 O 7 under various atmospheres and temperatures are also reported. The results provide a significant insight into the chemistry of group VII transition metals, investigate the potential use of benzotriazole as a reducing agent for metal productions, and demonstrate a successful convenient method for rhenium metal production, which could be applied to other refractory metals.

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Section: Resultsmentioning

confidence: 99%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: ■ Conclusionmentioning

confidence: 99%

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Thermal Analysis of Benzotriazolium Perrhenate and Its Implication to Rhenium Metal

et al. 2021

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“…Acid solutions are labeled with black line ( ____ ) and acid solutions with methanol are labeled in red line ( ____ ). Uv-visible spectra of rhenium soluble species and chloride ions in aqueous media are reported in few studies, which are enlisted in Table III (2,13,30,(37)(38). Uv-Visible spectra (black and red lines in Fig.…”

Section: Cyclic Voltammetry In Acidic Medium With or Without Methanolmentioning

confidence: 99%

Electrochemical Study of Metallic Rhenium in Methanol Acidic Aqueous Solutions

Orozco¹,

Rivera²

2022

ECS Trans.

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Cyclic voltammograms were performed in a window potential from -0.4 to 1.6 V, in solutions of a) H2SO4 0.5M, b) CH3OH 2 M + 0.5 M, c) HCl 0.145 M, d) CH3OH 2 M + HCl 0.145 M. In the sweeps towards anodic direction a soluble oxide is formed at potential superior to 1 V, which is electrodeposited in the sweeps towards cathodic direction. The electrodeposited surface is formed by Re(I) and Re(0) and anodic peaks (0.47 V and 0.71 V vs SHE) correspond to the formation of higher oxidation states (Re(I)→Re(II)→Re(VI)). Methanol affects the structure of anodic peaks separately of the presence of ions chlorides or sulfates. In both acids the soluble oxide is formed and also this specie is produced in sulfuric acid solutions with methanol. Contrariwise, in hydrochloric acid solutions with methanol the perrhenate is the predominant specie. We suggest new hydrogen bonding structures in this solution. Furthermore, we propose a new bonding structure when methanol is dissolve in sulfuric acid or hydrochloric acid solutions. This specie produces bands at 317 nm or 321 nm in the UV-visible spectra of soluble oxide. The high corrosion of metallic rhenium impedes its use as an anode for methanol electrooxidation

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