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Recovery method of selenium-germanium-sulfur glass

A recovery method and technology of chalcogenide glass, which is applied in the field of hydrometallurgy, can solve the problems affecting germanium grade and difficult recovery of selenium simple substance, etc., and achieve the effect of high recovery rate

Active Publication Date: 2018-06-12
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

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Problems solved by technology

[0003] However, in the process of oxidative leaching, the selenium compound has been oxidized into simple selenium, and the selenium produced at this time is difficult to recover
At the same time, more selenium in the raw material will be distilled out together with germanium tetrachloride during the chlorination distillation process, which will affect the grade of germanium

Method used

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  • Recovery method of selenium-germanium-sulfur glass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Selenium germanium chalcogenide glass contains 22% selenium and 12% germanium.

[0042] 700g of material was crushed and ball-milled through a 100-mesh sieve, and 2800ml of 31% hydrochloric acid was added to the reactor, and 700ml of 95% concentrated sulfuric acid was added at a rate of 28L / h. After the addition, start stirring, and then add the sieved material, the mass volume ratio is 1g:5ml. After adding the materials, turn on the heating and raise the temperature to 67°C; add the saturated sodium chlorate solution into the reactor at a rate of 3L / h. During the process of adding, control the reaction temperature at 71°C, and when the potential rises to 221mV, stop adding, cool down, and press filter to obtain the filter residue and the liquid after a selenium precipitation; the filter residue weighs 57g, which is crude selenium with a purity of 93.8%.

[0043] Control the reaction temperature at 79°C and keep it warm for 4h. After the heat preservation finishes, ad...

Embodiment 2

[0046] Selenium germanium chalcogenide glass contains 27% selenium and 19% germanium.

[0047]600g of material was crushed and ball-milled through a 100-mesh sieve, and 3000ml of 32% hydrochloric acid was added to the reactor, and 600ml of 96% concentrated sulfuric acid was added at a rate of 20L / h. After the addition, start stirring, and then add the sieved material, the mass volume ratio is 1g:6ml. After adding the materials, turn on the heating and raise the temperature to 69°C; add the saturated sodium chlorate solution into the reactor at a rate of 5L / h. During the addition, control the reaction temperature at 76°C, and when the potential rises to 277mV , stop adding, lower the temperature, and press filter to obtain a filter residue and a liquid after selenium precipitation; the filter residue is crude selenium with a purity of 97.1%, weighing 41g.

[0048] Control the reaction temperature at 80°C and keep it warm for 5h. After the heat preservation is finished, add 20...

Embodiment 3

[0051] Selenium germanium chalcogenide glass contains 20% selenium and 13% germanium.

[0052] 700g of the material was crushed and ball-milled through a 100-mesh sieve, and 2100ml of hydrochloric acid with a concentration of 32% was added to the reactor, and 700ml of concentrated sulfuric acid with a concentration of 98% was added at a rate of 8L / h. After the addition, start stirring, and then add the sieved material, the mass volume ratio is 1g:4ml. After adding the materials, turn on the heating and raise the temperature to 69°C. Add the saturated solution of sodium chlorate to the reactor at a rate of 5L / h; during the process of adding, control the reaction temperature at 79°C, and when the potential rises to 319mV, stop adding, cool down, and press filter to obtain the filter residue and a precipitate Selenium liquid; the filter residue is crude selenium with a purity of 98.3%, weighing 21g.

[0053] Control the reaction temperature to 80°C and keep it warm for 4h. Aft...

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Abstract

The invention provides a recovery method of selenium-germanium-sulfur. The recovery method comprises the following steps: S1) crushing the selenium-germanium-sulfur glass, then performing ball milling, and obtaining glass powder; S2) mixing the glass powder, hydrochloric acid and concentrated sulfuric acid, extracting, adding an oxidant in the extraction process until the potential rises to 200 to400 mV, filtering, and obtaining a solution after the primary selenium deposition and crude selenium; S3) performing the chlorination distillation for the solution after the primary selenium deposition, and obtaining a solution after the distillation and germanium tetrachloride; S4) mixing the solution after the distillation and a reducing agent, reacting, filtering, and obtaining crude selenium.Compared with the prior art, by controlling the potential in the oxidation extraction process, the oxidation process is controlled, so that the selenium in the selenium-germanium-sulfur glass is oxidized from bivalence to zero valence, the element selenium is obtained, the selenium and the germanium are effectively separated, the selenium can be recovered by virtue of various ways, and the recovery rate is higher.

Description

technical field [0001] The invention belongs to the technical field of hydrometallurgy, and in particular relates to a method for recovering selenium-germanium chalcogenide glass. Background technique [0002] At present, selenium-germanium-chalcogenide glass mostly recovers selenium and germanium by oxidation roasting and other methods, and there are few reports on simultaneous recovery of selenium and germanium by wet method, but there are mature processes for the separate recovery of selenium and germanium by wet method. The recovery of selenium germanium chalcogenide glass can recover germanium by chlorination distillation after fully oxidizing and leaching selenium germanium, and then recover selenium by adding reducing agent to the distillation raffinate. [0003] However, in the process of oxidative leaching, the selenium compound has been oxidized into simple selenium, and the selenium produced at this time is difficult to recover. Simultaneously, more selenium in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/02C01G17/04
CPCC01B19/02C01G17/04
Inventor 郑子健熊平陈辉殷亮朱刘
Owner 昆明先导新材料科技有限责任公司
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