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Method for purifying crude selenium through anhydrous ethanol

A technology of absolute ethanol and crude selenium, which is applied in the field of hydrometallurgical engineering, can solve the problems of long production cycle, high requirements for test conditions, and long time consumption, and achieve the effect of efficient extraction and purification

Pending Publication Date: 2019-01-18
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vacuum distillation can effectively separate impurities with high melting point and low saturated vapor pressure such as copper, silver, and gold, but it is difficult to remove impurities such as Te, Pb, and S to a low level; zone smelting is an effective method for purifying metals. But the production cycle is long, not suitable for mass production
Chemical methods include crude selenium oxidation and volatilization-sulfur dioxide reduction method, hydrogen selenide thermal decomposition method, sodium sulfite method, solvent extraction and ion exchange method, etc.; oxygen volatilization-sulfur dioxide reduction method requires high test conditions, complicated process and poor working conditions , pollute the environment; highly toxic gas hydrogen selenide will be produced in the process of purifying selenium by thermal decomposition of hydrogen selenide, so this method can only produce high-purity selenium in a small amount
The sodium sulfite method can effectively remove impurities that are difficult to remove by vacuum distillation. This method utilizes that selenium is soluble in hot sodium sulfite solution but impurities are insoluble. Disadvantages such as long time and extremely low recovery rate

Method used

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  • Method for purifying crude selenium through anhydrous ethanol
  • Method for purifying crude selenium through anhydrous ethanol
  • Method for purifying crude selenium through anhydrous ethanol

Examples

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Effect test

Embodiment 1

[0019] A method for purifying crude selenium with dehydrated alcohol, specifically comprises the following steps:

[0020] The crude selenium raw material is crushed, passed through a 50-mesh sieve, and then 300ml of 300g / L sodium sulfite solution is prepared and the crude selenium raw material with a purity of 90% is added to the reaction kettle at the same time according to the liquid-solid ratio of 15:1, and the temperature is controlled at 120°C. The stirring speed is 350r / min, the reaction is carried out under heating in an oil bath and magnetic stirring for 3 hours, and the selenium-containing leachate is obtained by filtration.

[0021] Use a measuring cylinder to measure excess absolute ethanol and add it to the sodium selenosulfate leaching solution, and immediately obtain selenium precipitate under the condition of stirring speed of 320r / min, and then filter, wash, and dry (60°C) to obtain refined selenium ; With reference to the People's Republic of China Nonferrous...

Embodiment 2

[0025] A method for purifying crude selenium with dehydrated alcohol, specifically comprises the following steps:

[0026] Crush the crude selenium raw material, pass through a 50-mesh sieve, prepare 300ml of 300g / L sodium sulfite solution and add the crude selenium raw material with a purity of 93% into the reaction furnace at the same time according to the liquid-solid ratio of 20:1. 300r / min, react for 2h under mechanical stirring, and filter to obtain sodium selenosulfate leaching solution.

[0027] Use a measuring cylinder to measure excess absolute ethanol and add it to the sodium selenosulfate leaching solution to obtain selenium precipitates, which are then filtered, washed, and dried (60°C) to obtain refined selenium; the obtained refined selenium refers to the nonferrous metal industry of the People's Republic of China According to the standards YS / T223-2007 and YS / T226.13-2009, the purity of refined selenium is detected by inductively coupled plasma mass spectrometr...

Embodiment 3

[0031] A method for purifying crude selenium with dehydrated alcohol, specifically comprises the following steps:

[0032] The coarse selenium raw material is pulverized, crosses 50 mesh sieves, the thick selenium raw material is processed, the sodium sulfite solution 300ml of preparation 300g / L and purity are 99% thick selenium raw material is that 9:1 is added in the reaction furnace simultaneously by liquid-solid ratio, control The temperature was 50° C., the stirring speed was 200 r / min, the reaction was performed under mechanical stirring for 1.5 h, and the sodium selenosulfate leaching solution was obtained by filtration.

[0033] Use a measuring cylinder to measure excess absolute ethanol and add it to the sodium selenosulfate leaching solution to obtain selenium precipitates, which are then filtered, washed, and dried (60°C) to obtain refined selenium; the obtained refined selenium refers to the nonferrous metal industry of the People's Republic of China According to t...

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Abstract

The invention discloses a method for purifying crude selenium through anhydrous ethanol, and belongs to the technical field of wet metallurgical engineering. The method comprises the steps that a sodium sulfite solution is used for leaching the crude selenium (containing 90%-99% of selenium), wherein the leaching temperature is 50-150 DEG C, the leaching time is 0.5-3 h, and the stirring speed is100-350 r / min; and after leaching, filtering is conducted to obtain a sodium selenosulphate leaching solution, the obtained sodium selenosulphate leaching solution and the excess anhydrous ethanol aremixed and stirred to obtain selenium precipitate, and finally the selenium precipitate is washed, filtered and dried to obtain fine selenium with the purity being 99.99%-99.999%. Metal impurities such as tellurium, lead, copper, silver and gold in leaching slag are further enriched. The anhydrous ethanol is adopted to precipitate the selenium from the sodium selenosulphate solution, thus efficient extraction and purification of the selenium are achieved, and no exhaust gases or waste residues are generated in the whole process.

Description

technical field [0001] The invention relates to a method for purifying crude selenium with absolute ethanol, and belongs to the technical field of hydrometallurgical engineering. technical background [0002] Selenium is a scattered metal, and its important position in the national economy and human health is becoming more and more prominent. Selenium has a wide range of applications, mainly used in electronic industries such as photoelectric cells, solar cells, and pigment industries. In terms of human health, selenium is one of the essential trace elements for the human body. Selenium-enriched foods have also received widespread attention, and they also play a key role in the synthesis of human anticancer drugs. The production of high-purity selenium has also been highly valued; for a long time, the selenium produced in my country is mainly industrial-grade products with a purity of more than 98%, which severely limits the development of high-tech new materials. Selenium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/02
CPCC01B19/02
Inventor 蒋文龙杨斌查国正刘大春徐宝强陈秀敏李一夫郁青春杨红卫田阳邓勇王飞熊恒杨佳曲涛孔令鑫郭新宇邓聚海黄大鑫周毅程明强高哲
Owner KUNMING UNIV OF SCI & TECH
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