Germanium separation and purification by leaching and precipitation

Abstract

In this research work, extraction and purification of germanium from zinc leach residues (ZLR) were investigated. The results of ICP, XRF, and atomic adsorption spectroscopy (AAS) tests show that contents of germanium, iron, lead, and zinc within the leaching residue were 105×10⁻⁶, 3.53%, 10.35%, and 8.8%, respectively. XRD results indicate that the main minerals were in different forms of sulfates (CaSO₄·2H₂O, PbSO₄ and ZnSO₄·6H₂O), silicate (SiO₂), and oxide (Fe₂O₃). Dissolution of leaching filter cake was carried out using 5 parameters and each in 4 levels (acid concentration, temperature, time, liquid-to-solid ratio, and stirring speed) by Taguchi method (L₁₆), and then optimization of the effective parameters by response surface method. Under optimum conditions, zinc and germanium dissolution efficiencies were 88.71% and 8%, respectively. Leaching tests with sulfuric acid (added di-ammonium oxalate monohydrate) and hydrochloric acid (HCl) on the residues obtained from previous-stage sulfuric acid dissolution, yielded germanium and iron recoveries of 83%, 88%, 40%, and 90%, respectively. Thus, leaching experiment with sulfuric acid (added di-ammonium oxalate monohydrate) was superior to that with hydrochloric acid due to high and low extraction amounts of germanium and iron, respectively. Precipitation experiments revealed that germanium purification with tannic acid presented a better result compared to sodium hydroxide and ammonia. Under optimum conditions, contents of germanium and iron in the solution after precipitation were 0.1505% and 14.7% with precipitation yields of 91% and 52%, respectively.

Keywords

experimental design / di-ammonium oxalate monohydrate / germanium / leaching / tannic acid

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