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An electrochemical process for preparing a compound comprising a metal or metalloid and a peroxide, ionic or radical species

a technology of peroxide and compound, applied in the direction of electrolysis process, electrode, electrolysis components, etc., can solve the problems of unsatisfactory ree demand, high polydisperse size and shape distribution, and the above described methods do not provide true, economically feasible recovery rates

Inactive Publication Date: 2018-01-25
VLAAMSE INSTELLING VOOR TECHNOLOGISCH ONDERZOEK NV VITO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention provides a process for efficiently isolating metal or metalloid ions from water soluble precursor compounds using an electrolyte. The process results in minimal conductivity variations in the electrolyte and can be operated in a continuous or batch-wise manner. This is achieved by adhesion or adsorption of cations containing the at least one metal element and / or metalloid element of the water soluble precursor compound onto the electrochemically active surface of the cathode and compensates for any unwanted variations in conductivity. A binary electrolyte can be added to increase the electrolytic conductivity and minimize the risk of a varying conductivity as a result of the removal of metal and / or metalloid ions.

Problems solved by technology

Regardless of the method used for their preparation many challenges have to be to overcome, like controlling particle growth, crystallinity, stability and reproducibility.
In a few cases, formation of nanocrystals with an average particle size below 100 nm has been observed, however these exhibit highly polydisperse (non-uniform) size and shape distributions.
A key measure to anticipate REE supply vulnerabilities is recycling from end-of-life products; yet recycling possibilities are far from sufficient to meet the REE demand.
However, the above described methods do not provide true, economically feasible recovery rates, where possible in a form which permits re-use of the metal.
The existing extraction methods for extracting REE or other critical metals from aqueous matrixes, e.g. to meet regulatory requirements, are insufficient and need to be adapted to provide a commercially interesting product.
The alkaline conditions in which the reaction is carried out cause particle diameters to increase, and obtaining the metal hydroxides as particles with a uniform desired particle diameter is hard to achieve.
Moreover, the process involves the use of an organic electrolyte and is therefore not suitable for example for recovering metal ions from aqueous solutions.
As a result, formation and growth of particles of the reaction product in the pores of the porous electrochemically active material will be limited by the dimensions of those pores.
Although the electrochemically active surface of the cathode may contain adsorbed reactive radicals and / or adsorbed oxidant gas, and although the water based electrolyte may contain some dissolved oxidant gas, this will usually not be enough to ensure full recovery of all metal or metalloid ions present in the electrolyte.
In general the concentration of the water soluble compound will not be higher than 10 g / liter as the efficiency of the process can hardly be improved at higher concentrations.

Method used

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  • An electrochemical process for preparing a compound comprising a metal or metalloid and a peroxide, ionic or radical species
  • An electrochemical process for preparing a compound comprising a metal or metalloid and a peroxide, ionic or radical species
  • An electrochemical process for preparing a compound comprising a metal or metalloid and a peroxide, ionic or radical species

Examples

Experimental program
Comparison scheme
Effect test

example 2

[0201]Independent electrodes were tested as gas-diffusion cathodes, in presence of air at the gas compartment (to provide O2 for its reduction to H2O2, its polyatomic ions or radical). The reagents presented in Table A were dissolved in demineralized water and the pH of the solution where the pH was adjusted to approximately 4.

TABLE AComposition of catholyte in demineralized water.ChemicalQuantityChemical nameformula(mg · L−1)1Cerium nitrate hexahydrateCe(NO3)3•6H2O3502Dysprosium nitrate x hydrateDy(NO3)3•xH2O803Erbium nitrate pentahydrateEr(NO3)3•5H2O534Europium nitrate pentahydateEu(NO3)3•5H2O65Gadolinium nitrateGd(NO3)3•6H2O59hexahydrate6Holmium nitrateHo(NO3)3•5H2O18pentahydrate7Lanthanum nitrateLa(NO3)3•6H2O159hexahydrate8Lutetium nitrate hydrateLu(NO3)3•xH2O69Neodymium nitrateNd(NO3)3•6H2O206hexahydrate10Praseodymium nitratePr(NO3)3•6H2O51hexahydrate11Samarium nitrateSm(NO3)3•6H2O53hexahydrate12Terbium nitrate hexahydrateTb(NO3)3•6H2O1213Thulium nitrate pentahydrateTm(NO3)3•5H...

example 3

[0207]The composition of the electrolyte was identical to that explained for example 1, but lanthanum nitrate was used instead of cerium nitrate, in concentrations of 0 ppm, 100 ppm, 500 ppm, 1000 ppm and 5000 ppm.

[0208]The initial pH and conductivity of the catholytes containing the different concentrations of the metal are disclosed in Table b. The operational volume of the catholyte in each experiment was 125 mL.

TABLE bMeasured pH and conductivity of the catholyteswith different concentrations of lanthanum nitrateLa(NO3)3•6H2O by the start of experimentation.Concentration (ppm)010050010005000CatholytepH2.542.152.702.782.76Conductivity51.051.650.450.352(mS · cm−1)AnolytepH2.82.82.742.742.74Conductivity49.749.749.849.849.8(mS · cm−1)

[0209]The concentration of lanthanum was quantitatively analyzed by means of ICP-MS.

[0210]A colourless solution was formed when dissolving the chemicals. Air was supplied to the gas compartment. After 2 h of processing at constant polarization condition...

example 4

[0211]The composition of the electrolyte was identical to that explained for example 1 but instead of cerium nitrate a boric acid was supplied in the catholyte. The concentration of boric acid was kept constant for all experiments (5 g·L−1). The effect of the polarization potential was evaluated. The following potentials vs. the reference electrode were compared: −0.350 V, −0.550 V, −0.750 V, −0.950 V. The operational volume of the catholyte in each experiment was 125 mL.

TABLE DpH and conductivity of the catholyte at the startof experimentation at different cathode potentials.Applied potential (V vs Ag / AgCl 3M KCl)−0.150−0.350−0.550−0.750−0.950CatholytepH2.672.632.512.512.76Conductivity47.147.447.247.446.9(mS · cm−1)AnolytepH2.742.742.82.82.8Conductivity49.849.849.749.749.7(mS · cm−1)

[0212]From the changes in the pH and conductivity, especially of the catholyte, it can be observed that the same trend found in previous examples was observed; this is, the pH significantly increased th...

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Abstract

An electrochemical process is for recovering a metal element or a metalloid element or a mixture of two or more thereof from at least one water soluble precursor compound containing the metal element or a metalloid element or two or more thereof, in the form of one or more nano particles, in particular nano crystals of at least one reaction product. The process includes supplying the water soluble precursor compound to a water-based catholyte of a cathode compartment of an electrochemical cell, equipped with a cathode containing a gas diffusion electrode, adjusting the pH of the catholyte, supplying at least one oxidant gas to the gas diffusion electrode, and subjecting the cathode to an electrochemical potential to cause reduction of the at least one oxidant gas.

Description

[0001]The present invention relates to electrochemical process for recovering a metal element or a metalloid element or a mixture of two or more thereof from at least one water soluble precursor compound comprising the metal element or a metalloid element or two or more thereof, in the form of one or more nano particles of at least one reaction product, according to the preamble of the first claim.[0002]The present invention further relates to nano particles, in particular nano crystals obtained with that process and to a device for carrying out the process of the invention.BACKGROUND OF THE INVENTION[0003]Nano particles and their composites exhibit unconventional electronic, optical, magnetic and chemical properties with respect to bulk phase particles and macroscopic crystals. Hence, they offer new or improved properties for application in a wide variety of fields ranging from catalysis, cosmetics, textiles, nano-electronics, high-tech components and defense gadgets, to pharmaceut...

Claims

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Application Information

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IPC IPC(8): C25B1/30C25B11/00
CPCC25B1/30C25B11/00C25B1/00
Inventor DOMINGUEZ BENETTON, XOCHITLALVAREZ GALLEGO, YOLANDAPORTO-CARRERO, CHRISTOFGIJBELS, KATRIJNRAJAMANI, SUNITA
Owner VLAAMSE INSTELLING VOOR TECHNOLOGISCH ONDERZOEK NV VITO
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