Direct electrochemical synthesis of metal alcoholates

Shreider, V. A.; Turevskaya, E. P.; Kozlova, N. I.; Turova, Nataliya

doi:10.1007/bf00952176

Cited by 8 publications

(5 citation statements)

References 7 publications

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“…5 In 1972 the electrochemical synthesis of tantalum ethoxide by anodic dissolution of tantalum in ethanol in the presence of NH 4 Cl as an electroconductive additive was patented. 6 Since then, tantalum ethoxide was prepared by Shreider et al, 7 Turova et al, 8 and our teams 9,10 using the electrochemical method. The electrochemical technique appeared to have been successfully employed in Russia for the commercial production of alkoxides of Y, Ti, Zr, Nb, Ta, Mo, W, Cu, Ge, Sn, and other metals.…”

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confidence: 98%

Electrochemical Behavior of Tantalum in Anhydrous Ethanol

Yang

Cai

et al. 2010

J. Electrochem. Soc.

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The electrochemical behaviors of Ta in Et4NCl ethanol solutions were investigated using potentiodynamic polarization, cyclic voltammetry, and potentiostatic current–time transient techniques, complemented with a scanning electron microscope (SEM). The potentiodynamic anodic polarization curves did not exhibit an active dissolution region due to the presence of a thin oxide film on the electrode surface, which was followed by pitting corrosion as a result of passivity breakdown by the aggressive attack of Cl− anions. SEM images confirmed the existence of pits on the electrode surface. The pitting potential (Enormalb) decreased with the increase in solution temperature, but increased with increasing potential scan rate. The potentiostatic current–time transients showed that the incubation time slightly decreased with increasing Et4NCl concentrations. The pitting growth current density agreed well with Hills’s model.

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confidence: 98%

Electrochemical Behavior of Tantalum in Anhydrous Ethanol

Yang

Cai

et al. 2010

J. Electrochem. Soc.

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“…In addition, the necessary reagents are scarce, and the reactions involve multistep processes and are accompanied by various side processes which contaminate the products and decrease their yields. 9 Electrochemical dissolution of metals in absolute alcohols with a supporting electrolyte seems a promising synthesis method of metal alkoxides due to simplicity and high productivity as well as its continuous and non-polluting character. 10 In 1972, the electrochemical synthesis of Ti, Ta, Si alkoxides was patented.…”

Section: Introductionmentioning

confidence: 99%

Electrochemical Synthesis of Zirconium n-Butoxide

et al. 2017

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Zirconium n-butoxide was successfully synthesized using electrochemical method and characterized by IR and 1 H-NMR spectra. The influence of various factors on the cell voltage of electrosynthesis process was studied. The cell voltage increased with an increase of electrode distance and current density, but decreased with the increasing Bu n 4 NBr concentration and solution temperature. The ideal conditions for electrosynthesis of zirconium n-butoxide were obtained. The resulting zirconium n-butoxide solution was purified by distillation and n-hexane extraction. Infrared spectra conformed to chemical bonds excellently, and the peak area ratio of nuclear magnetic resonance coincided with number ratio of hydrogen atoms in Zr(OC 4 H 9 ) 4 . The purity was close to 99.99%.

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“…In addition, the yield is low. 7 Electrochemical dissolution of metals in absolute alcohols containing a supporting electrolyte has proved to be a promising synthesis method of metal alkoxides. 8 Many researchers synthesized niobium, zirconium and hafnium alkoxides using electrochemical method.…”

Section: Introductionmentioning

confidence: 99%

Anodic Dissolution Behavior of Zirconium in n-Butanol Solutions Containing Bu<sup>n</sup><sub>4</sub>NBr

2016

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Anodic dissolution of zirconium in Bu n 4 NBr-containing n-butanol solutions was investigated using cyclic voltammetry, linear sweep voltammetry and potentiostatic current-time transient and scanning electron microscopy (SEM). Zirconium did not exhibit active dissolution due to passivation in the potential region of 0.2 to 1.2 V vs. SCE. The zirconium dissolution in passive state was under mass transfer control. Pitting corrosion took place as a result of passivity breakdown by Br − anions and the typical steady-state pitting potential was between 1.55-1.60 V vs. SCE in n-butanol solutions containing 0.08 M Bu n 4 NBr. SEM images confirmed the occurrence and the intensification of pits with an increase of potential. Increasing Bu n 4 NBr concentration accelerated the pit nucleation and growth. The reaction order leading to pit nucleation process was 1.0 with respect to bromide anions. The dissolution of zirconium in n-butanol solution produced Zr(OC 4 H 9 ) 4 .

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Direct electrochemical synthesis of metal alcoholates

Cited by 8 publications

References 7 publications

Electrochemical Behavior of Tantalum in Anhydrous Ethanol

Electrochemical Behavior of Tantalum in Anhydrous Ethanol

Electrochemical Synthesis of Zirconium n-Butoxide

Anodic Dissolution Behavior of Zirconium in n-Butanol Solutions Containing Bu<sup>n</sup><sub>4</sub>NBr

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