| Summary: | This work presents the results of laboratory scale tests of the CARBOFLUOREX (CARBOnate FLUORide EXtraction) process – a novel technology for the recovery of U and Pu from the solid fluorides residue (fluorination ash) of Fluoride Volatility Method (FVM) reprocessing of spent nuclear fuel (SNF). To study the oxidative leaching of U from the fluorination ash (FA) by Na2CO3 or Na2CO3–H2O2 solutions followed by solvent extraction by methyltrioctylammonium carbonate in toluene and purification of U from the fission products (FPs) impurities we used a surrogate of FA consisting of UF4 or UO2F2, and FPs fluorides with stable isotopes of Ce, Zr, Sr, Ba, Cs, Fe, Cr, Ni, La, Nd, Pr, Sm. Purification factors of U from impurities at the solvent extraction refining stage reached the values of 104–105, and up to 106 upon the completion of the processing cycle. Obtained results showed a high efficiency of the CARBOFLUOREX process for recovery and separating of U from FPs contained in FA, which allows completing of the FVM cycle with recovery of U and Pu from hardly processed FA. Keywords: Fluorination ash, Uranium tetrafluoride, Uranyl fluoride, Oxidative leaching, Solvent extraction, Quaternary ammonium compounds, Methyltrioctylammonium carbonate
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