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, ...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(CaSO_4·2H_2O, PbSO_4 and ZnSO_4·6H__2O), silicate(SiO_2), and oxide(Fe_2O_3). 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(L_(16)), 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.展开更多
Reduction smelting of the bismuth oxide residue from pressure leaching of bismuth sulfide was investigated in the FeO-SiO_2-CaO ternary slag system.The results show that all the recovery ratios of Bi,Ag,Cu and Pb incr...Reduction smelting of the bismuth oxide residue from pressure leaching of bismuth sulfide was investigated in the FeO-SiO_2-CaO ternary slag system.The results show that all the recovery ratios of Bi,Ag,Cu and Pb increase with the increase of reductive coal proportion,reaction temperature and time,while too much reductive coal would help Fe enter metal phase;CaO/SiO_2and Fe O/SiO_2 of the chosen slag system should be 0.5-0.75 and 1.25-1.75,respectively,for the reason that the slag system has the optimum mobility and is beneficial for the recovery of metals.The corresponding optimum conditions are determined as follows:the added coal proportion is 7%of the leaching residue,CaO/SiO_2 mass ratio in the chosen slag system is 0.5 and FeO-SiO_2 is 1.5,the reaction temperature is 1300°C and the reaction time is 40 min.Under the above conditions,the recovery ratios of Bi,Ag,Cu and Pb are 99.6%,99.8%,97.0%and 97.3%,respectively.展开更多
文摘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(CaSO_4·2H_2O, PbSO_4 and ZnSO_4·6H__2O), silicate(SiO_2), and oxide(Fe_2O_3). 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(L_(16)), 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.
基金Project(134414) supported by the Postdoctoral Funded Program of Central South University,China
文摘Reduction smelting of the bismuth oxide residue from pressure leaching of bismuth sulfide was investigated in the FeO-SiO_2-CaO ternary slag system.The results show that all the recovery ratios of Bi,Ag,Cu and Pb increase with the increase of reductive coal proportion,reaction temperature and time,while too much reductive coal would help Fe enter metal phase;CaO/SiO_2and Fe O/SiO_2 of the chosen slag system should be 0.5-0.75 and 1.25-1.75,respectively,for the reason that the slag system has the optimum mobility and is beneficial for the recovery of metals.The corresponding optimum conditions are determined as follows:the added coal proportion is 7%of the leaching residue,CaO/SiO_2 mass ratio in the chosen slag system is 0.5 and FeO-SiO_2 is 1.5,the reaction temperature is 1300°C and the reaction time is 40 min.Under the above conditions,the recovery ratios of Bi,Ag,Cu and Pb are 99.6%,99.8%,97.0%and 97.3%,respectively.
