A method for preparing high-purity selenium by a crude selenium wet method

A high-purity, wet purification technology, applied in the direction of element selenium/tellurium, etc., can solve the problems of high-purity selenium having no commonality, low recovery rate, and difficulty in finding, so as to shorten the selenium purification process, reduce production costs, and reduce limitations sexual effect

Inactive Publication Date: 2019-07-19
三门峡市有色金属质量科学研究所
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] At present, Germany, Chile, and Japan are the main producers of high-purity selenium in foreign countries, but the key technologies of their purification processes are kept strictly confidential, and it is difficult to find relevant reports from published literature.
Domestic selenium purification processes mainly include oxidation-adsorption precipitation method, neutralization-hydrolysis combined method, and ion exchange-extraction method. These methods have problems such as long process flow, high cost, serious pollution, and low recovery rate, making it difficult to produce on a large scale.
Chinese patent application CN102627262 (application number 201210129139.7) "Method for extracting high-purity selenium from by-products of high-temperature scarlet production" discloses a method for extracting high-purity selenium from by-products of high-temperature scarlet production, mainly for ceramic industry Wrap waste, remove silicon, zirconium, cadmium, sulfur and other interfering substances that coexist with cadmium selenide, and extract high-purity selenium, which has no commonality with crude selenium wet purification to prepare high-purity selenium
"Purification and Preparation of High Purity Selenium" (Materials Research and Application, Wu Hao et al., Vol.4, No.4, Dec.2010) discloses a purification process combining oxidative combustion-vacuum distillation, the raw material is 99.9% selenium, no purification process for 80-90% high impurity crude selenium

Method used

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  • A method for preparing high-purity selenium by a crude selenium wet method
  • A method for preparing high-purity selenium by a crude selenium wet method

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) First weigh 200g of high-impurity crude selenium after drying, slurry it with 200ml of water, turn on the stirring, and slowly add 500ml of sodium hydroxide solution with a mass fraction of 35%, and the leaching time is 1.5h to ensure that the crude selenium is completely dissolved and leached ;

[0031] (2) Use hydrochloric acid with a mass fraction of 5% to adjust the pH of the alkaline infusion to 6.8, then add 100 g of sodium sulfide, stir and mix, and let stand for 1 hour to filter and remove impurities to obtain the alkaline infusion;

[0032] (3) Continue to adjust the pH to 1.2 with hydrochloric acid with a mass fraction of 10% in the alkaline immersion solution, age for 2.5 hours, take the supernatant to detect the selenium content in the solution (≤0.15g / l), the selenium precipitation is complete, and the solid-liquid separation obtains the selenium selenium;

[0033] (4) Oxidatively leaching refined selenium with 40% sodium sulfite solution, controlling ...

Embodiment 2

[0036] (1) First, 260g of high-impurity crude selenium containing 15% water is slurried with 300ml of water, turned on and stirred, and slowly added to 500ml of sodium hydroxide solution with a mass fraction of 40%, and the leaching time is 2 hours to ensure that the crude selenium is completely dissolved and leached;

[0037] (2) Use hydrochloric acid with a mass fraction of 10% to adjust the pH of the alkaline immersion solution to 7.0, then add 110g of sodium sulfide, stir and mix, and let it stand for 1 hour to filter and remove impurities to obtain the alkaline immersion solution;

[0038] (3) Use hydrochloric acid with a mass fraction of 15% to adjust the pH to 1.0 in the alkaline immersion solution, stir evenly, age for 3.0 hours, take the supernatant to detect the selenium content in the solution (≤0.15g / l), the selenium precipitation is complete, solid liquid separation to obtain refined selenium;

[0039] (4) Oxidatively leaching fine selenium with 45% sodium sulfite...

Embodiment 3

[0042] (1) First, 300g of high-impurity coarse selenium with 20% water content is mixed with 400ml of water into a slurry, and 500ml of 45% sodium hydroxide solution is added in small amounts to the slurry of coarse selenium several times, and stirred while adding, the reaction The time is 2.5h to ensure that the crude selenium is completely dissolved and leached;

[0043] (2) Use hydrochloric acid with a mass fraction of 15% to adjust the pH of the alkaline immersion solution to 7.0, then add 120g of sodium sulfide, stir and mix, and let it stand for 1 hour to filter and remove impurities to obtain the alkaline immersion solution;

[0044] (3) Continue to adjust pH to 1.0 with hydrochloric acid with a mass fraction of 20% in the alkaline immersion solution. After stirring evenly, age for 3.0 hours, take the supernatant to test the selenium content in the solution (≤0.15g / l), the selenium precipitation is complete, solid liquid separation to obtain refined selenium;

[0045] ...

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Abstract

The invention discloses a method for preparing high-purity selenium through wet-process purification of crude selenium. The method comprises the following steps: a, slowly adding crude selenium into a sodium hydroxide solution at a uniform speed, wherein a liquid-solid mass ratio is 3-5: 1, reaction time is 1.5 to 2 h and complete dissolving and leaching of crude selenium are ensured; b, adjusting a pH value to 6.5 to 7.0 by using hydrochloric acid, adding sodium sulfide, then carrying out uniform mixing under stirring and carrying out standing to remove impurities; c, adjusting the pH value of an alkaline leaching solution obtained in the previous step to 1.0 to 1.5, carrying out ageing for 2.5 to 3 h and then carrying out solid-liquid separation after complete precipitation of selenium; d, oxidizing leached fine selenium by using a sodium sulfite solution, carrying out sufficient stirring and then successively carrying out standing and filtering so as to obtain a selenium-rich solution; and e, slowly adding sulfuric acid into the selenium-rich solution, and successively carrying out acidification and reduction, filtering, washing and drying so as to prepare high-purity selenium. The method provided by the invention realizes preparation of high-purity selenium through two-step leaching and wet-process purification of crude selenium, shortens the purification flow of selenium, improves recovery rate, reduces production cost and mitigates limitation of large-scale production.

Description

technical field [0001] The invention relates to the field of high-purity rare metal preparation, in particular to a process for preparing high-purity selenium by wet purification of crude selenium. Background technique [0002] At present, Germany, Chile, Japan, etc. mainly produce high-purity selenium in foreign countries, but the key technology of their purification process is strictly kept secret, and it is difficult to find relevant reports from published literature. Domestic selenium purification processes mainly include oxidation-adsorption precipitation method, neutralization-hydrolysis combined method, and ion exchange-extraction method. These methods have problems such as long process flow, high cost, serious pollution, and low recovery rate, making it difficult to produce on a large scale. Chinese patent application CN102627262 (application number 201210129139.7) "Method for extracting high-purity selenium from by-products of high-temperature scarlet production" di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/02
CPCC01B19/02C01P2006/80
Inventor 吴冰乌新平徐娟南立志孙加法孟伟粉李广友王志麟刘亚芳张慧娟
Owner 三门峡市有色金属质量科学研究所
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