Convenient Routes for the Preparation of Barium Permanganate and other Permanganate Salts

Kótai, László; Sajó, István E.; Gács, István; Sharma, Pradeep K.; Banerji, Kalyan K.

doi:10.1002/zaac.200700142

Cited by 12 publications

(18 citation statements)

References 22 publications

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“…Chemiresistive responses of the permanganate-functionalized devices to the various VOCs are summarized in Figure ; chemiresistive responses of analogous devices simply acidified with dilute H 2 SO 4 to the same VOCs are also shown for comparison as a negative control and exhibit no significant changes in resistance. Control experiments with devices fabricated from pyridinium permanganate and SWCNTs without the P4VP could not be conducted because pyridinium permanganate has only been reported in a polymer-supported form and discrete compounds are not known. , We were also unable to identify a suitable solvent system that was inert to KMnO 4 in which both KMnO 4 could be dissolved and SWCNTs could be dispersed sufficiently well to fabricate chemiresistors from a KMnO 4 –SWCNT composite via drop casting methods.…”

Section: Resultsmentioning

confidence: 99%

“…Control experiments with devices fabricated from pyridinium permanganate and SWCNTs without the P4VP could not be conducted because pyridinium permanganate has only been reported in a polymersupported form and discrete compounds are not known. 52,53 We were also unable to identify a suitable solvent system that was inert to KMnO 4 in which both KMnO 4 could be dissolved and SWCNTs could be dispersed sufficiently well to fabricate chemiresistors from a KMnO 4 −SWCNT composite via drop casting methods.…”

Section: Chemistry Of Materialsmentioning

confidence: 99%

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Surface-Anchored Poly(4-vinylpyridine)–Single-Walled Carbon Nanotube–Metal Composites for Gas Detection

2016

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A platform for chemiresistive gas detectors based upon single-walled carbon nanotube (SWCNT) dispersions stabilized by poly(4-vinylpyridine) (P4VP) covalently immobilized onto a glass substrate was developed. To fabricate these devices, a glass substrate with gold electrodes is treated with 3-bromopropyltrichlorosilane. The resulting alkyl bromide coating presents groups that can react with the P4VP to covalently bond (anchor) the polymer–SWCNT composite to the substrate. Residual pyridyl groups in P4VP not consumed in this quaternization reaction are available to coordinate metal nanoparticles or ions chosen to confer selectivity and sensitivity to target gas analytes. Generation of P4VP coordinated to silver nanoparticles produces an enhanced response to ammonia gas. The incorporation of soft Lewis acidic Pd2+ cations by binding PdCl2 to P4VP yields a selective and highly sensitive device that changes resistance upon exposure to vapors of thioethers. The latter materials have utility for odorized fuel leak detection, microbial activity, and breath diagnostics. A third demonstration makes use of permanganate incorporation to produce devices with large responses to vapors of volatile organic compounds that are susceptible to oxidation.

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Section: Resultsmentioning

confidence: 99%

Section: Chemistry Of Materialsmentioning

confidence: 99%

Surface-Anchored Poly(4-vinylpyridine)–Single-Walled Carbon Nanotube–Metal Composites for Gas Detection

2016

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“…Therefore, a chloride ion has to be introduced into the inner coordination sphere of the cobalt in the absence of a permanganate ion-for example, with the preparation of [Co(NH 3 ) 5 Cl]Cl 2 (compound 4) [14]-and the outer sphere chloride ions have to be exchanged with permanganate ions, such as occurred with the perrhenate ions in the preparation of compound 3-Re [15,16]. A possible reaction route is the reaction of [Co(NH 3 ) 5 Cl]SO 4 [14] with barium permanganate [17][18][19][20]; however, this method was not used due to the relatively low solubility of compound 3-Mn in water that causes problems in the separation of compound 3-M from the insoluble barium sulfate by-product. The reaction of compound 4 and an excess of NaMnO 4 in a 40% aq.…”

Section: Synthesis and Properties Of Compound 3-mnmentioning

confidence: 99%

Multi-Centered Solid-Phase Quasi-Intramolecular Redox Reactions of [(Chlorido)Pentaamminecobalt(III)] Permanganate—An Easy Route to Prepare Phase Pure CoMn2O4 Spinel

et al. 2022

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We synthesized and structurally characterized the previously unknown [Co(NH3)5Cl](MnO4)2 complex as the precursor of CoMn2O4. The complex was also deuterated, and its FT-IR, far-IR, low-temperature Raman and UV-VIS spectra were measured as well. The structure of the complex was solved by single-crystal X-ray diffraction and the 3D-hydrogen bonds were evaluated. The N-H…O-Mn hydrogen bonds act as redox centers to initiate a solid-phase quasi-intramolecular redox reaction even at 120 °C involving the Co(III) centers. The product is an amorphous material, which transforms into [Co(NH3)5Cl]Cl2, NH4NO3, and a todorokite-like solid Co-Mn oxide on treatment with water. The insoluble residue may contain {Mn4IIIMnIV2O12}n4n-, {Mn5IIIMnIVO12}n5n- or {MnIII6O12}n6n- frameworks, which can embed 2 × n (CoII and/or CoIII) cations in their tunnels, respectively, and 4 × n ammonia ligands are coordinated to the cobalt cations. The decomposition intermediates decompose on further heating via a series of redox reactions, forming a solid CoIIMIII2O4 spinel with an average size of 16.8 nm, and gaseous N2, N2O and Cl2. The CoMn2O4 prepared in this reaction has photocatalytic activity in Congo red degradation with UV light. Its activity strongly depends on the synthesis conditions, e.g., Congo red was degraded 9 and 13 times faster in the presence of CoMn2O4 prepared at 550 °C (in air) or 420 °C (under N2), respectively.

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“…Melting points (m.p., °C) were taken on a microhot stage apparatus Boetius PHMK 05 and are uncorrected. BaMnO 4 was synthesized according to the work of Kótai et al [ 33 ].…”

Section: Methodsmentioning

confidence: 99%

“…For the synthesis of the imidazole ring, we applied the Weidenhagen reaction [31], according to the experimental procedure described by Baldwin et al [32] and introducing some modifications at the work-up stage. The aldehydes 2a-c were obtained from the corresponding alcohols (1a-c) by mild oxidation with BaMnO4 that has been freshly synthesized following a published procedure [33]. The aldehyde 2d was obtained from 2b by heating for 15 h at 100 • C in 48% HBr, and therefore the corresponding methanol derivative 1d was not studied experimentally.…”

Section: Synthesis and Nmr Measurements In Solutionmentioning

confidence: 99%

13C CPMAS NMR as a Tool for Full Structural Description of 2-Phenyl Substituted Imidazoles That Overcomes the Effects of Fast Tautomerization

et al. 2020

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Tautomerization of 2-phenylimidazolecarbaldehydes has not been studied in detail so far, although this process is a well-known phenomenon for imidazole derivatives. That is why we focus our study on a series of 2-phenylimidazolecarbaldehydes and their parent alcohols that were synthesized and studied by detailed 1H and 13C NMR in solution and in the solid state. The apparent problem is that the fast tautomerization impedes the full structural description of the compounds by conventional 13C NMR measurements. Indeed, the 13C NMR spectra in solution exhibit poor resolution, and in most cases, signals from the imidazole ring are not detectable. To avoid this problem, we used 13C CP-MAS NMR as an alternative spectroscopic method for unambiguous spectroscopic characterization of the studied series of 2-phenylimidazoles. The data were analyzed in combination with quantum chemical DFT-GIAO methods by considering the tautomerization process and the intermolecular interactions. The DFT (B3LYP/6-31G(d,p)) calculations allowed to identify and suggest the preferred tautomer in the gas phase and in DMSO solvent, which for alcohols are (2-phenyl-1H-imidazol-4-yl)methanol and its analogs, and for the aldehydes are the 2-phenyl-1H-imidazole-5-carbaldehydes. The gas-phase calculated energy differences between the two possible tautomeric forms are in the range 0.645–1.415 kcal/mol for the alcohols and 2.510–3.059 kcal/mol for the aldehydes. In the DMSO solvent, however, for all compounds, the calculated energy differences go below 1.20 kcal/mol. These data suggest that both tautomeric forms of the studied 2-phenylimidazoles can be present in solution at room temperature. Our data from detailed 2D NMR measurements in the solid state (1H-13C HETCOR and 1H-1H double-quantum coherence MAS NMR) suggested that also in the solid state both tautomers coexist in different crystalline domains. This fact does not obscure the 13C CP-MAS NMR spectra of the studied 2-phenyl substituted imidazoles and suggests this spectroscopic method as a powerful tool for a complete structural description of tautomeric systems with aromatic conjugation.

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Convenient Routes for the Preparation of Barium Permanganate and other Permanganate Salts

Cited by 12 publications

References 22 publications

Surface-Anchored Poly(4-vinylpyridine)–Single-Walled Carbon Nanotube–Metal Composites for Gas Detection

Surface-Anchored Poly(4-vinylpyridine)–Single-Walled Carbon Nanotube–Metal Composites for Gas Detection

Multi-Centered Solid-Phase Quasi-Intramolecular Redox Reactions of [(Chlorido)Pentaamminecobalt(III)] Permanganate—An Easy Route to Prepare Phase Pure CoMn2O4 Spinel

13C CPMAS NMR as a Tool for Full Structural Description of 2-Phenyl Substituted Imidazoles That Overcomes the Effects of Fast Tautomerization

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