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Recovery system and method for germanium-containing liquid in high-purity germanium dioxide production

A germanium dioxide and recovery method technology, applied in chemical instruments and methods, germanium halide, neutralization water/sewage treatment, etc., can solve the problems of low leaching rate, high adjustment precision, easy kiln formation in post-treatment production process, etc.

Inactive Publication Date: 2020-03-27
四川高锗再生资源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. The three-step sedimentation is adjusted to different pH values ​​so that ferric chloride can fully hydrolyze and absorb germanium in the liquid phase, and finally it can be recycled by pressure filtration to make slag; it needs to adjust the pH value many times, and it needs to be adjusted with high accuracy and control The process is difficult; the post-treatment production and processing of recovered germanium-containing materials exist in the kiln dehydration process, which is easy to kiln, and the hardness after dehydration is high, and the leaching rate of the post-processing production process after crushing is not high;
[0005] 2. Adjust the pH value of the solution to 1~2, then add tannin to precipitate germanium, and obtain tannin germanium after filtration. Although the recovery effect is good, the cost is extremely high

Method used

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  • Recovery system and method for germanium-containing liquid in high-purity germanium dioxide production

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Adopt above-mentioned method to reclaim germanium-containing liquid in the production of high-purity germanium dioxide, wherein the auxiliary agent adopted in the S2 step is a mixture of quicklime and gypsum powder, in parts by weight, the ratio of quicklime and gypsum powder is 2:1, wherein The dosage of quicklime is 2.5g per liter of the solution to be reacted.

[0040] This method only needs to test the pH at intervals, and it can be used after it meets the requirements, avoiding repeated adjustments to the pH value, and the volume of each liquid mixed does not need to be accurate, and can be realized within a rough range; using this method to obtain The requirements for the equipment for the filter cake in the post-treatment dehydration are not high, and the requirements for the post-treatment after using ferric chloride or tannin recovery are high, and it is easy to break, and it is convenient for leaching and distillation; and the method has simple steps, convenien...

Embodiment 2

[0042] The above method is used to recover the germanium-containing liquid in the production of high-purity germanium dioxide, wherein the auxiliary agent used in the S2 step is magnesium chloride.

[0043] The auxiliary agent of this embodiment can precipitate germanium in the germanium-containing liquid, but the applicant found that when using this auxiliary agent, in the S6 step, crystallization easily occurs in the connecting pipe between the rear liquid circulation temporary storage tank and the tail gas absorption liquid storage tank , leading to blockage, which is difficult to deal with.

Embodiment 3

[0045] The above method is used to recover the germanium-containing liquid in the production of high-purity germanium dioxide, wherein the auxiliary agent used in the S2 step is magnesium oxide.

[0046] The effect of the auxiliary agent in this embodiment is similar to that of embodiment 2, and there is also the problem of crystallization blockage.

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Abstract

The invention provides a recovery system and method for germanium-containing liquid in high-purity germanium dioxide production and relates to the technical field of germanium-containing liquid recovery. The recovery system comprises a germanium tetrachloride hydrolyzed liquid storage tank, a tail gas absorption liquid storage tank, a water tank, a liquid mixing tank, a reaction tank, a sedimentation tank and a filter press. The germanium tetrachloride post-hydrolysis liquid storage tank, the tail gas absorption liquid storage tank and the water tank are respectively communicated with the liquid mixing tank, the liquid mixing tank, the reaction tank, the sedimentation tank and the filter press are sequentially communicated to be used for treating an aqueous solution step by step, in the whole production process, only the pH needs to be tested at intervals, the system can be used after the requirement is met, the repeated adjustment of the pH value is avoided, the mixing volume of all liquid does not need to be accurate, and the effect can be achieved within a rough range.

Description

technical field [0001] The invention belongs to the technical field of germanium-containing liquid recovery, and in particular relates to a recovery system and method for germanium-containing liquid in the production of high-purity germanium dioxide. Background technique [0002] The germanium-containing liquid is the output liquid and the absorption liquid of the tail gas absorption system during the hydrolysis of germanium tetrachloride in the high-purity germanium dioxide production system; the output liquid during the hydrolysis of germanium tetrachloride is distilled water and high-purity germanium tetrachloride in a specific The product under certain conditions; the absorption liquid of the tail gas absorption system is a mixture of caustic soda and water; among them, germanium has great economic recovery value and is a necessary product in the production process of high-purity germanium dioxide. [0003] At present, there are roughly two processes for recovering the l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/04C02F11/122C02F11/12C01G17/04C02F101/20
CPCC01G17/04C02F1/5236C02F1/5281C02F1/66C02F9/00C02F11/12C02F11/122C02F2001/007C02F2101/20
Inventor 李忠政
Owner 四川高锗再生资源有限公司
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