The invention relates to the technical field of
precious metal refining, in particular to a preparation method of high-purity
rhodium powder, which comprises the following steps: S1, mixing a
raw material with
rhodium content greater than or equal to 1% with caustic alkali and
alkali metal peroxide, and carrying out alkali fusion treatment to obtain filter residues; s2, dissolving the filter residues with
aqua regia to obtain filtrate. And S3, controlling the
rhodium concentration and oxidation potential in the filtrate, adding
ammonium chloride to obtain filtrate, and continuously adding
sulfamic acid into the filtrate to obtain filtrate. And S4, dissolving the filter residue with an acid solution to obtain a filtrate. And S5, adding
ammonium sulfite into the filtrate to obtain a new filtrate. S6, alkali liquor is continuously added, filter residues are obtained, the filter residues are dissolved, and new filtrate is obtained. And S7, adding
ammonia water into the filtrate to obtain rhodium precipitate, and calcining and post-
processing to obtain high-purity rhodium
powder. The preparation method is generally suitable for low-grade and high-grade raw materials, the process is short, complex pretreatment is not needed, impurities such as
ruthenium and
iridium can be effectively removed, and the product purity is larger than or equal to 99.95%.