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A kind of method that recovers copper indium gallium selenide from waste material containing copper indium gallium selenide

A copper indium gallium selenide and copper recovery technology, which is applied in the field of non-ferrous metal metallurgy, can solve the problems of high cost and complicated process, and achieves the effects of low recovery cost, simple process, and easy production and application.

Active Publication Date: 2016-01-13
ZHUZHOU SMELTER GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the defects of the existing copper indium gallium selenium recovery process of copper, indium, gallium and selenium, which are complex and costly, the present invention provides a simple method and low cost copper indium gallium selenium recovery method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Using 3 kg of CIGS waste as raw material, the composition of the raw material is: 19.8% by weight of copper, 25.4% by weight of indium, 5.7% by weight of gallium, and the balance being selenium.

[0063] The first step is to crush CIGS to obtain 120-mesh CIGS powder.

[0064] In the second step, the above powder is leached with nitric acid with a mass percentage concentration of 30% to obtain a leachate, and the mass ratio of nitric acid to powder is controlled to be 4:1, the leaching temperature is 60°C, and the leaching time is 1 hour. Copper, The leaching rate of indium, gallium and selenium is 100%.

[0065] The third step is to adjust the acidity of the above leaching solution with sodium hydroxide, and stabilize it for 15 minutes when the pH reaches 1, so as to obtain the acid adjustment solution.

[0066] The fourth step, when the temperature of the above-mentioned acid-adjusting solution reaches 50°C, calculate the theoretical amount of the reducing agent thiou...

Embodiment 2

[0073] Using 3 kg of CIGS waste as raw material, the composition of the raw material is: 19.8% by weight of copper, 25.4% by weight of indium, 5.7% by weight of gallium, and the balance being selenium.

[0074] The first step is to crush CIGS to obtain 150-mesh CIGS powder.

[0075] In the second step, the above-mentioned powder is leached with nitric acid with a mass percentage concentration of 20% to obtain a leachate, and the mass ratio of nitric acid to powder is controlled to be 6:1, the leaching temperature is 70°C, and the leaching time is 3 hours. Copper, The leaching rate of indium, gallium and selenium is 100%.

[0076] The third step is to adjust the acidity of the above leaching solution with potassium hydroxide, and stabilize it for 25 minutes when the pH reaches 1.5, so as to obtain the acid adjustment solution.

[0077]In the fourth step, when the temperature of the acid-adjusting solution reaches 60°C, the required reducing agent Na is calculated according to ...

Embodiment 3

[0084] Using 3 kg of CIGS waste as raw material, the composition of the raw material is: 19.8% by weight of copper, 25.4% by weight of indium, 5.7% by weight of gallium, and the balance being selenium.

[0085] The first step is to crush CIGS to obtain 200-mesh CIGS powder.

[0086] In the second step, the above powder is leached with nitric acid with a mass percentage concentration of 30% to obtain a leachate, and the mass ratio of nitric acid to powder is controlled to be 8:1, the leaching temperature is 85°C, and the leaching time is 5 hours. Copper, The leaching rate of indium, gallium and selenium is 100%.

[0087] The third step is to adjust the acidity of the above leaching solution with sodium carbonate, and stabilize it for 30 minutes when the pH reaches 3, so as to obtain the acidification solution.

[0088] In the fourth step, when the temperature of the above-mentioned acid-adjusting solution reaches 70°C, the required reducing agent SO is calculated according to ...

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Abstract

The invention provides a method for recycling copper, indium, gallium and selenium from indium gallium selenium wastes containing copper. The method comprises the following steps: smashing indium gallium selenium to form powder; leaching the powder in a nitric acid so as to obtain a nitric acid leaching liquid; adding a reducing agent into the nitric acid leaching liquid so as to obtain crude selenium and a reducing liquid in a reducing manner; adding alkali into the reducing liquid and regulating pH to reach 10 to 14 so as to obtain an alkali leaching liquid and alkali leaching residues; neutralizing or electrolyzing the alkali leaching liquid with an acid so as to obtain gallium hydroxide or pure gallium; leaching the alkali leaching residues with a leaching agent so as to obtain ammonia leaching residues and an ammonia leaching liquid; reducing the ammonia leaching liquid with the reducing agent so as to obtain copper powder; and leaching the ammonia leaching residues with the acid and adding the reducing agent for replacement so as to obtain crude indium. When the recycling is carried out by utilizing the method, the indium can be simply and efficiently recycled while the copper, the gallium and the selenium can be efficiently recycled at the same time. Thus, the process procedures are simplified. The method is simple and convenient to operate, has no special requirement on equipment and realizes effective reduction in process production cost.

Description

technical field [0001] The invention belongs to the field of nonferrous metal metallurgy, and in particular relates to a method for recovering copper indium gallium selenide from waste materials containing copper indium gallium selenium. Background technique [0002] Copper indium gallium selenide (CIGS) thin-film solar cells have high photoelectric efficiency and have good development potential. Its production methods include vacuum sputtering method, distillation method and non-vacuum coating method. No matter which production method is used, some copper indium gallium selenide waste will be produced during the production process. In addition to heavy metal copper, these waste materials contain It also contains rare metals such as indium, gallium and selenium. In order to facilitate the sustainable utilization of rare metals such as indium, gallium and selenium and heavy metal copper, they need to be separated and recycled separately to facilitate further recycling and en...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/00C22B15/00C22B58/00C01B19/02
CPCY02P10/20
Inventor 林文军刘景文廖贻鹏刘一宁戴慧敏刘敏
Owner ZHUZHOU SMELTER GRP
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