Method for extracting indium and germanium from pyrometallurgical crucible residues by whole-wet method

An all-wet, crucible technology, applied in the field of comprehensive recovery of germanium and non-ferrous metal smelting and extraction of indium, can solve the problems of lower recovery rate, unfavorable leaching and separation of indium and germanium, unfavorable germanium recovery, etc., and achieves low environmental pollution and high recovery. rate effect

Inactive Publication Date: 2010-09-08
云南天浩稀贵金属股份有限公司
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Problems solved by technology

But zinc pyrometallurgy crucible slag usually contains germanium, after sulfuration roasting, the leaching rate of germanium is only 30-50%, which is unfavorable for the recovery of germanium; Most of it turns into ferric iron after roasting, which is not conducive to the leaching and separation of indium germanium
In addition, the above two pretreatment methods will melt out part of the lead water, disperse the indium and germanium, increase the recovery process and cost, and reduce the low recovery rate.

Method used

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  • Method for extracting indium and germanium from pyrometallurgical crucible residues by whole-wet method
  • Method for extracting indium and germanium from pyrometallurgical crucible residues by whole-wet method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take crucible scum as raw material, its composition is Pb 28.30%, Zn 8.12%, Ge 1.36%, In 0.96%, Ag 4267g / T, Fe 28.19%, the raw material is ground, all sieved 120 mesh, and stirred at room temperature , leached with 1.0M dilute sulfuric acid for 12 hours, the liquid-solid ratio was 5:1, and the terminal acidity was 11g / L. The leaching solution contains In860mg / L, Zn18.68g / L, and Ge 0mg / L. The dilute sulfuric acid leaching residue is oxidized and leached with sulfuric acid with a concentration of 5%, the liquid-solid ratio is 5:1, the reaction temperature is 70°C, and MnO with 1 times the feeding amount is evenly added 2 , Reaction time 6h, terminal acidity pH=3.0. The leaching solution contains germanium 2.48g / L and indium 2mg / L. The leaching rate of indium in dilute acid leaching is 40.31%, germanium is 0%; the leaching rate of germanium in oxide leaching is 80.24%, and indium is 0%. The first two stages of leaching can leach indium and germanium respectively. Oxida...

Embodiment 2

[0015] Take 674 kg of sieved 120-mesh material, and the grades of each element are Pb31.76%, Zn8.55%, Ge1.85%, In9481g / T, Ag3592.8g / T, Fe31.82%. Dilute sulfuric acid leaching: final acid (calculated as sulfuric acid) 11g / L, add 300 kg of sulfuric acid, stir and leaching at room temperature for 12 hours, and obtain a leaching solution of 3.85m 3 , containing indium 690mg / L, containing germanium 3mg / L; oxidation leaching: stirring and leaching at a temperature of 80°C for 6 hours, adding 700 kg of manganese powder, and the final acidity pH=2.5, and the volume of the leachate was 3.93m 3 , the leach solution contains germanium 2.49g / L, and indium content=5mg / L; chlorination salt leaching: add 240 kg of sodium chloride, add 220 kg of sulfuric acid, and the reaction temperature is >90°C to obtain a leach solution of 3.91m 3 , the acidity (sulfuric acid) of the leach solution is 67g / L, and the solution contains In882mg / L and Ge568mg / L. Dilute acid leaching and oxidation leaching ca...

Embodiment 3

[0017] Take 864 kg of sieved 120-mesh material, and the grades of each element are Pb 28.70%, Zn12.23%, Ge0.82%, In1.49%, Ag4367g / T, Fe33.81%. Dilute sulfuric acid leaching: final acid (calculated as sulfuric acid) 13g / L, 400 kg of sulfuric acid was added, stirred and leached at room temperature for 12 hours, and the leachate was 4.86m 3 , containing indium 1.02g / L, containing germanium 5mg / L; oxidation leaching: stirring and leaching at a temperature of 75°C for 6 hours, adding 900 kg of manganese powder, and the final acidity pH=3.0, resulting in a leachate volume of 4.70m 3 , the leaching solution contains germanium 1.18g / L, and indium=0mg / L; chlorination salt leaching: add 310 kg of NaCl, add H 2 SO 4 300 kg, reaction temperature > 90°C, leaching solution 4.56m 3 , the acidity of the leaching solution (sulfuric acid meter) 62g / L, In1.64g / L, Ge303mg / L. Three-stage leaching, leaching rate of In96.65%, Ge97.88%, dilute acid leaching, oxidation leaching, indium and germaniu...

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Abstract

The invention relates to a non-ferrous metal metallurgy and comprehensive recovery technology, in particular to a method for extracting indium and germanium from pyrometallurgical crucible residues by a whole-wet method, belonging to the technical field of non-ferrous metal metallurgy. The method comprises the following steps: grinding and sieving the crucible residues, and then leaching the indium by dilute sulphuric acid with the density of 0.5-1.0M according to the mass ratio of liquid to solid of 5-3:1; adding MnO2 the weight of which is 0.8-1.5 times of that of the dilute sulphuric acid to dilute sulphuric acid-leaching residues, and then leaching germanium by utilizing sulfuric acid with the density of 2-3M according to the ratio of liquid to solid of 5-3:1 in an oxidation manner; leaching the remaining indium and germanium from the oxidation-leaching residues by adopting a C1-1 solution with the density of 4-8wt% in a chlorination manner, keeping the ratio of liquid to solid be 5:1, meanwhile controlling the acidity be 60-80g / L with sulfuric acid; and recovering the leached indium in each segment by an extraction method, precipitating the leached germanium with tannin, and finally calcining to obtain germanium concentrate. The method has less environmental pollution; most part of germanium and indium can be respectively recovered in a leaching manner, wherein the indium can be recovered as well as the germanium; and higher recovery rate can be maintained.

Description

technical field [0001] The invention relates to a comprehensive recovery technology for nonferrous metal smelting, in particular to a method for extracting indium and germanium from pyrometallurgy crucible slag by using a full wet method, and belongs to the technical field of nonferrous metal smelting. technical background [0002] Since the zinc calcine used in pyrometallurgy contains scattered metal indium and germanium, it will be enriched in hard zinc during the zinc distillation process, and will be enriched in the crucible slag during the treatment of hard zinc. , the metal indium content is 0.10-2.0%, and the germanium content is between 0.30-2.0%. Indium and germanium are high-value scattered metals. It has high economic recovery value. [0003] If the general crucible slag contains only indium, it can be pretreated by sulfuration and roasting in the prior art, and then wet leached, so that the indium can have a higher leaching rate. But zinc pyrometallurgy crucib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/08C22B58/00C22B41/00
Inventor 叶志清
Owner 云南天浩稀贵金属股份有限公司
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