Method for separating and recovering selenium in chalcogenide glass waste

A technology for separation and recovery of chalcogenide glass, applied in the field of hydrometallurgy, which can solve problems such as low recovery rate, sulfur dioxide pollution, and large flue gas volume, and achieve the effects of low cost, simple equipment, and short process

Active Publication Date: 2018-05-15
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in this method, selenium is dispersedly recovered in several different processes, the recovery rate is low and the purity is not easy to control; and there are problems such as large flue gas volume, sulfur dioxide pollution, and high energy consumption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] (1) The chalcogenide glass waste containing 38.6% of selenium, 12.5% ​​of germanium, and 12.6% of arsenic is crushed and ball-milled by crushing ball milling equipment, and passed through a 200-mesh sieve to obtain a powder with a particle size of less than 75 μm.

[0061] (2) Weigh 100g of the powder obtained in step (1), add 300mL of 500g / L NaOH solution, heat up to 90°C, and react for 4h at a stirring speed of 600r / min, then add 400mL of water, and continue the heat preservation reaction After 1 h, cool and filter to obtain 800 mL of mixed solution.

[0062] Sampling and inspection, using ICP-MS to detect Ge, As, and Se in the above mixed solution, the contents are: Ge15.432g / L, As 15.671g / L, Se 47.62g / L; after calculation, the germanium leaching rate is 98.8% , The leaching rate of arsenic is 99.5%, and the leaching rate of selenium is 98.7%.

[0063] (3) Measure 500mL of the mixed solution obtained in step (2), slowly add concentrated sulfuric acid at a stirring s...

Embodiment 2

[0068] (1) The chalcogenide glass waste containing 38.6% of selenium, 12.5% ​​of germanium, and 12.6% of arsenic is crushed and ball-milled by crushing ball milling equipment, and passed through a 200-mesh sieve to obtain a powder with a particle size of less than 75 μm.

[0069] (2) Weigh 100g of the powder obtained in step (1), add 400mL of 400g / L NaOH solution, heat up to 80°C, and react for 5h at a stirring speed of 600r / min, then add 400mL of water, and continue the heat preservation reaction After 1 h, 895 mL of mixed solution was obtained by cooling and filtration.

[0070] Sampling and inspection, using ICP-MS to detect Ge, As, and Se in the above mixed solution, the contents are respectively: Ge13.757g / L, As 14.036g / L, Se 42.74g / L; after calculation, the leaching rate of germanium is 98.5% , The leaching rate of arsenic is 99.7%, and the leaching rate of selenium is 99.1%.

[0071] (3) Measure 500mL of the mixed solution obtained in step (2), slowly add concentrated ...

Embodiment 3

[0076] (1) The chalcogenide glass waste containing 38.6% of selenium, 12.5% ​​of germanium, and 12.6% of arsenic is crushed and ball-milled by crushing ball milling equipment, and passed through a 200-mesh sieve to obtain a powder with a particle size of less than 75 μm.

[0077] (2) Weigh 100g of the powder obtained in step (1), add 500mL of 500g / L NaOH solution, heat up to 70°C, and react for 6h at a stirring speed of 600r / min, then add 400mL of water and continue the heat preservation reaction After 1 h, cool and filter to obtain 990 mL of mixed solution.

[0078] Sampling was sent for inspection, and Ge, As, and Se in the above mixed solution were detected by ICP-MS, and their contents were respectively: Ge 12.5g / L, As 12.52g / L, Se 38.72g / L; after calculation, the germanium leaching rate was 99.0% , The leaching rate of arsenic is 98.4%, and the leaching rate of selenium is 99.3%.

[0079] (3) Measure 500mL of the mixed solution obtained in step (2), slowly add concentrat...

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Abstract

The invention provides a method for separating and recovering selenium in chalcogenide glass waste. The method comprises the following steps: (a) crushing and sieving the chalcogenide glass waste to obtain powder with particle size of less than 75mu m; (b) mixing the powder obtained in the step (a) with a strong alkaline solution, carrying out alkaline extracting, and filtering to obtain a mixed solution; (c) mixing the mixed solution obtained in the step (b) with concentrated sulfuric acid and an oxidizing agent, carrying out controlled-potential oxidation and selenium precipitation, and filtering to respectively obtain filtrate and a crude selenium product, wherein the potential in the controlled-potential oxidation and selenium precipitation is 150-300mV. Compared with the prior art, the method firstly controls the particle size of the chalcogenide glass waste to be less than 75mu m, and adopts the controlled-potential oxidation and selenium precipitation after the alkaline extracting is finished, so that the selenium elementary substance is obtained by carrying out low valence oxidation on the selenium, and the selenium is effectively separated from germanium, arsenic, and thelike. The method for separating and recovering the selenium in the chalcogenide glass waste is high in recovery rate; the selenium obtained by using the method is good in purity; the method does not need large equipment for performing fire roasting, thus being low in energy consumption; furthermore, the method is free from pollution caused by harmful gases.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for separating and recovering selenium in chalcogenide glass waste. Background technique [0002] Chalcogenide glass is a special glass material with excellent infrared transmission performance, which is widely used in the fields of phase change optical storage, solar cells and optical waveguides. Ge-As-Se chalcogenide glass is one of the most concerned basic systems among many infrared chalcogenide glass systems. It has attracted much attention for its excellent internal optical quality, good wave forming performance, and not easy to devitrify. [0003] During the preparation, processing and use of Ge-As-Se chalcogenide glass, some wastes and substandard products are usually produced, which contain a relatively high content of Se, which can be recycled as secondary resources. At present, the sulfated roasting method is commonly used in the prior art to reclaim ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/02C22B7/00C22B41/00
CPCC01B19/02C22B7/008C22B41/00Y02P10/20
Inventor 陈辉熊平殷亮朱刘
Owner 昆明先导新材料科技有限责任公司
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