Method for efficiently recycling germanium

A high-efficiency, germanium slag technology, applied in the field of metallurgy, can solve the problems of difficult to adapt to environmental protection requirements, short equipment life, high corrosion resistance requirements, and achieve accelerated neutralization rate and germanium leaching efficiency, improve leaching efficiency, and short process. Effect

Inactive Publication Date: 2018-02-23
CHENZHOU FENGYUE ENVIRONMENTAL PROTECTION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the lead-zinc-copper smelting process, when the germanium in the raw material is high, the germanium can be enriched in soot or replacement slag and other materials. When dealing with these materials with high germanium content, the current commonly used process, one is through regular Germanium is leached by pressure or high-pressure oxygen leaching, germanium is absorbed and enriched by tannin extract, germanium dioxide is recovered by distillation, germanium in the leached slag is recovered to soot through a fuming furnace, and leached again; the comprehensive recovery rate of germanium in this method is only 90% , at the same time increased fuming treatment, resulting in long process and high production cost
The second is to add fluoride or nitrate during atmospheric pressure leaching to increase the leaching rate of germanium; the leaching rate of germanium in this method can reach 90-95%, but due to the addition of fluoride or nitrate, the corrosion resistance of the equipment is high. The service life of the equipment is short, the operating environment is relatively harsh, and it is difficult to meet the requirements of environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The method for efficiently reclaiming germanium comprises the following steps:

[0034] (1) Using germanium slag as raw material, crushing the germanium slag, using a ball mill for ball milling, the mass ratio of the ball to material is 32:1, the grinding balls are steel balls with a diameter of 4mm, the ball mill speed is 300rpm, and the ball mill is 130 mesh;

[0035] (2) The germanium slag obtained in step (1) is acid-leached with sulfuric acid solution, and microwaves are introduced to strengthen the leaching. ℃, the time is 0.7h, while leaching, add leaching aid-potassium oxalate (the amount of potassium oxalate is 6% of the quality of germanium slag) and oxidant-hydrogen peroxide (the concentration of hydrogen peroxide is 28%, and its addition is 12% of the quality of germanium slag ), control the final acid concentration at 80g / L, obtain pickling slag and pickling solution after pickling is completed; after testing, the content of germanium in the pickling soluti...

Embodiment 2

[0040] The method for efficiently reclaiming germanium comprises the following steps:

[0041] (1) Using germanium slag as raw material, crushing the germanium slag, using a ball mill for ball milling, the mass ratio of the ball to material is 40:1, the grinding ball is a steel ball with a diameter of 4mm, the ball mill speed is 350rpm, and the ball mill is 160 mesh;

[0042] (2) The germanium slag obtained in step (1) is acid-leached with sulfuric acid solution, and microwave is introduced to strengthen the leaching. ℃, the time is 0.8h, while leaching, add leaching aid-potassium oxalate (the amount of potassium oxalate is 7% of the quality of germanium slag) and oxidant-hydrogen peroxide (the concentration of hydrogen peroxide is 30%, and its addition is 11% of the quality of germanium slag ), control the final acid concentration at 90g / L, and obtain pickling slag and pickling solution after pickling is completed; after testing, the content of germanium in the pickling solut...

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Abstract

The invention belongs to the field of metal recycling and particularly discloses a method for efficiently recycling germanium. The method comprises the following steps that germanium slag is crushed and subjected to ball milling into a material of 130-180 meshes; a sulfuric acid solution is used for microwave acid leaching, a leaching aid agent and an oxidizing agent are added while leaching is conducted, the final acid concentration is controlled to be within 70-90 g / L, and acid-leached slag and acid-leached solution are obtained after acid leaching; and a potassium oxide is added into the solution, two times of neutral leaching are conducted, first-time filter residues and second-time filter residues are roasted at the temperature of 380-480 DEG C for 2.5-4 h, thus, a coarse germanium dioxide is obtained, and after the coarse germanium dioxide is subjected to the working procedures of chloridizing distillation, rectifying and hydrolyzing, a high-purity germanium dioxide is prepared.The method is easy and convenient to operate, the technology is simple, and the process is short; and only one time of acid leaching and the two times of neutral leaching need to be conducted, and thecomprehensive recycling rate of germanium reaches 98.6% or above.

Description

technical field [0001] The invention belongs to the technical field of metallurgy and relates to metal recovery, in particular to a method for efficiently recovering germanium. Background technique [0002] Germanium is an important semiconductor material used in the manufacture of transistors and various electronic devices. Germanium is a dispersed element, which is mainly dispersed in nature and associated with polymetallic deposits. At present, germanium is mainly extracted from lead-zinc nucleated copper sulfide ores in industry. [0003] In the lead-zinc-copper smelting process, when the germanium in the raw material is high, the germanium can be enriched in soot or replacement slag and other materials. When dealing with these materials with high germanium content, the current commonly used process, one is through regular Germanium is leached by pressure or high-pressure oxygen leaching, germanium is absorbed and enriched by tannin extract, germanium dioxide is recover...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B1/02C22B41/00
CPCC22B1/02C22B7/007C22B41/00Y02P10/20
Inventor段良洪廖谨鹏刘伟郭远贵肖尚
OwnerCHENZHOU FENGYUE ENVIRONMENTAL PROTECTION TECH