Method for recovery germanium from germanium-containing flue dust

A germanium fume and obtained technology, applied in the field of germanium recovery, can solve the problems of low germanium recovery rate, long process flow, environmental pollution, etc., and achieve the effects of high recovery rate, simplified process process, and reduced production cost

Inactive Publication Date: 2013-06-26
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These processes have long process flow, low recovery rate of germanium, high energy consumption, high cost, and serious environmental pollution.

Method used

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  • Method for recovery germanium from germanium-containing flue dust

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Crush and sieve 500g of germanium dust containing 0.05% Ge to -200 mesh;

[0030] (2) According to the liquid-solid ratio (L / kg) of 0.5:1, stir and mix the water and the germanium dust obtained in step (1) evenly;

[0031] (3) In the mixture obtained in step (2), add industrial sulfuric acid with a mass concentration of 80% according to the liquid-solid ratio (L / kg) of acid to germanium fumes of 2.5:1, and keep stirring at 90°C for 2 hours until until no more gas is produced in the slurry;

[0032] (4) Under the condition of stirring at 60°C, press H 2 o 2 The liquid-solid ratio (L / kg) to germanium fumes is 1:1. Add H with a mass concentration of 50% to the slurry obtained in step (3) at a speed of 1L / min. 2 o 2 , the adding time is controlled at 0.8h until H 2 o 2 Complete decomposition without bubbles;

[0033] (5) Filter the slurry obtained in step (4), add industrial hydrochloric acid with a mass concentration of 70% to the filtered clear liquid according...

Embodiment 2

[0036] (1) Crush and sieve germanium dust to -200 mesh;

[0037] (2) According to the liquid-solid ratio (L / kg) of 0.8:1, stir and mix the water and the germanium dust obtained in step (1) evenly;

[0038] (3) In the mixture obtained in step (2), add industrial sulfuric acid with a mass concentration of 70% according to the liquid-solid ratio (L / kg) of acid to germanium fumes of 2:1, and continue stirring at 88°C for 2.5h until Until no more gas is produced in the slurry;

[0039] (4) Under the condition of stirring at 50°C, press H 2 o 2 The liquid-solid ratio (L / kg) to germanium fumes is 0.8:1. Add H with a mass concentration of 40% to the slurry obtained in step (3) at a speed of 1.1 L / min. 2 o 2 , the addition time is controlled at 0.5h until H 2 o 2 Complete decomposition without bubbles;

[0040] (5) Filter the slurry obtained in step (4), and add industrial hydrochloric acid with a mass concentration of 60% to the filtered clear liquid according to the liquid-sol...

Embodiment 3

[0043] (1) Crush and sieve germanium dust to -200 mesh;

[0044] (2) According to the liquid-solid ratio (L / kg) of 1:1, stir and mix the water and the germanium dust obtained in step (1) evenly;

[0045] (3) In the mixture obtained in step (2), add industrial sulfuric acid with a mass concentration of 50% according to the liquid-solid ratio (L / kg) of acid to germanium fumes of 1.5:1, and continue stirring at 85°C for 2.2h until Until no more gas is produced in the slurry;

[0046] (4) Under the condition of stirring at 70°C, press H 2 o 2 The liquid-solid ratio (L / kg) to germanium fumes is 0.5:1. Add H with a mass concentration of 30% to the slurry obtained in step (3) at a speed of 1.2 L / min. 2 o 2 , the addition time is controlled at 1h until H2 o 2 Complete decomposition without bubbles;

[0047] (5) Filter the slurry obtained in step (4), and add industrial hydrochloric acid with a mass concentration of 45% to the filtered clear liquid according to the liquid-solid r...

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Abstract

The invention provides a method for recovering germanium from germanium-containing flue dust. According to the invention, germanium flue dust is crushed and sieved, and is well mixed with water by stirring; industrial sulfuric acid is added, and continuous stirring is carried out under a temperature of 85-90 DEG C, until no more gas is produced in the material slurry; under stirring and under a temperature of 50-70 DEG C, H2O2 is added, until H2O2 is completely decomposed and no bubble appears; the obtained material slurry is filtered; industrial hydrochloric acid is added; heating is carried out, and distillation is carried out for 2-4h with distilled water as an absorbent, such that a distillate liquid I is obtained; re-distillation is carried out, such that a distillate liquid II is obtained; the distillate liquid II is hydrolyzed; and filtering and bake-drying are carried out, such that high-purity germanium dioxide powder is obtained. The flue dust processing method provided by the invention has the advantages of simple technology, easy operation, low investment, high recovery rate, and the like. The method has high comprehensive utilization rate upon germanium flue dust. Besides germanium, valuable metals such as zinc, lead, and silver can be recycled.

Description

technical field [0001] The invention relates to a method for recovering germanium from germanium-containing fumes, and belongs to the technical field of extraction of nonferrous rare metals and comprehensive utilization of industrial waste. Background technique [0002] During the smelting of germanium-containing lead-zinc oxide ore and the combustion of germanium-containing lignite, most of the germanium exists in the form of soot. As for the valuable metals in the dust, after carbon reduction, they all become simple substances or low-priced compounds, and the content of germanium in them generally ranges from 0.05 to 5.0%. As for the method of reclaiming germanium from the soot, at present, the soot is sieved and then leached with sulfuric acid, and then the pH of the leachate is adjusted to 2 to 3, and then the germanium is precipitated with tannic acid or glue, and the germanium is precipitated and baked. After dry roasting, germanium concentrate is obtained; or germani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/02C22B3/08C22B3/22C22B41/00
CPCY02P10/20
Inventor 郑东升肖松
Owner KUNMING UNIV OF SCI & TECH
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