At present, the processing of refractory gold–arsenic sulphide concentrates is becoming more relevant due to the depletion of rich crude ore reserves. In the process of the nitric acid leaching of arsenic sulphide minerals, solutions are formed containing 20–30 g/L of arsenic (III). Since market demand for arsenic compounds is limited, such solutions are traditionally converted into poorly soluble compounds. This paper describes the investigation of precipitating arsenic sulphide from nitric acid leaching solutions of refractory sulphide raw materials of nonferrous metals containing iron (III) ions using sodium hydrosulphide with a molar ratio of NaHS/As = 2.4–2.6, which is typical for pure model solutions without oxidants. The work studied the effect of temperature, the pH of the solution and the consumption of NaHS and seed crystal on this process. The highest degree of precipitation of arsenic (III) sulphide (95–99%) from nitric acid leaching solutions containing iron (III) ions without seed occurs with a pH from 1.8 to 2.0 and a NaHS/As molar ratio of 2.8. The introduction of seed crystal significantly improves the precipitation of arsenic (III) sulphide. An increase in seed crystal consumption from 0 to 34 g/L in solution promotes an increase in the degree of transition of arsenic to sediment from 36.2 to 98.1% at pH = 1. According to SEM/EDS and XRF sediment data, from the results of experiments on the effect of As2S3 seed crystal consumption, acidity and molar ratio of NaHS/As on the precipitation of arsenic (III) sulphide and the Fetotal/Fe2+ ratio in the final solution, it can be concluded that the addition of a seed accelerates the crystallisation of arsenic (III) sulphide by increasing the number of crystallisation centres; as a result, the deposition rate of As2S3 becomes higher. Since the oxidation rate of sulphide ions to elemental sulphur by iron (III) ions does not change significantly, the molar ratio of NaHS/As can be reduced to 2.25 to obtain a precipitate having a lower amount of elemental sulphur and a high arsenic content similar to that precipitated from pure model solutions.

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An integrated two-stage metallurgical process has been developed to process concentrates from the Olimpiadinskoe deposit, which contain high levels of antimony and arsenic. The optimal parameters for the alkaline sulfide leaching process of the initial concentrate from the Olimpiadinskoe deposit were determined to achieve the maximum extraction of antimony at a 99% level. The recommended parameters include an L:S ratio of 4.5:1, a sodium sulfide concentration of 61 g/L, a sodium hydroxide concentration of 16.5 g/L, a duration of 3 h, and a temperature of 50 °C. A synergistic effect of co-processing alkaline sulfide leach cakes with sulfuric and nitric acids was observed. The pre-treatment step reduced the nitric acid composition by converting carbonates into gypsum and increased the arsenic extraction by 15% during subsequent nitric acid leaching. The laboratory research on the nitric acid leaching of decarbonized cake established the key parameters for the maximum iron and arsenic extraction in solution (92% and 98%, respectively), including an L:S ratio of 9:1, a nitric acid concentration of 6 mol/L, and a time of 90 min. Full polynomial equations for the iron and arsenic extraction from the decarbonized cake were derived. The model demonstrated a high relevance, as evidenced by the determination coefficients (R2) of 96.7% for iron and 93.2% for arsenic. The technology also achieved a high gold recovery rate of 95% from the two-stage alkaline sulfide and nitric acid leach cake. Furthermore, the maximum deposition of arsenic from the nitrate leach solution in the form of insoluble As2S3 was determined to be 99.9%. A basic technological flow sheet diagram for processing the flotation gold–antimony concentrate from the Olimpiadinskoe deposit was developed, including two stages: the production of metallic antimony and the gold extraction from the nitric leach cake.

An integrated two-stage metallurgical technology has been developed for processing concentrates from the Olimpiadinskoe deposit with high antimony and arsenic content. The parameters of the alkaline sulphide leaching process of the initial concentrate of the Olimpiadinskoe deposit, providing maximum extraction of antimony in solution at 99% level have been recommended. The L:S ratio = 4,5:1; the concentration of sodium sulphide - 61 g/L; the concentration of sodium-hydroxide – 6,5 g/L; the duration – 3 hours; the temperature – 50 °C. A synergistic effect of alkaline sulphide leach cakes co-processing by sulphuric and nitric acids has been determined. Pre-treatment allows to reduce the composition of nitric acid by converting the carbonates into gypsum and increases the extraction of arsenic by 15 % at the following nitric leaching. Laboratory research of nitric acid leaching of decarbonized cake allowed to set the basic parameters for maximum iron and arsenic extraction in solution (92 and 98 %): the L:S ratio =9:1; the concentration of nitric acid – 6 mol/L; the time – 90 min. The full polynomial equations for iron and arsenic extraction from decarbonised cake have been derived. The model is relevant since the value the determination coefficients for iron and arsenic R2 were 96,7 and 93,2 %. The high value of gold recovery from the cake of two-stage alkaline sulphide and nitric acid leach cake at 95 % has been established. The maximum value of arsenic deposition from the nitrate leach solution in the form of the insoluble deposition As2S3 99,9 %. A basic technological flowsheet diagram for flotation gold-antimony processing for the Olimpiadinskoe deposit has been developed; it includes two redistributions: production of metallic antimony and gold extraction from the nitric leach cake.