A kind of preparation method of high-purity selenium
A technology of high-purity selenium and crude selenium, applied in the direction of elemental selenium/tellurium, etc., can solve the problems of low direct yield of high-purity selenium, difficult separation of selenium and tellurium, etc., and achieve the effect of simple process, high purity of selenium, and high-efficiency removal
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[0025] The invention provides a kind of preparation method of high-purity selenium, comprises the following steps:
[0026] Slurrying the coarse selenium slag to obtain selenium mud; the mass percentage of Se in the coarse selenium slag is 60-95%;
[0027] Adjusting the pH value of the selenium slurry, adding an oxidizing agent to the oxidation potential, followed by precipitation reaction and filtration to obtain primary selenium; the oxidation potential is 400-700mV;
[0028] Melting the primary selenium to obtain a selenium melt;
[0029] The selenium melt is subjected to vacuum distillation to obtain high-purity selenium.
[0030] In the present invention, unless otherwise specified, each component is a commercially available product well known to those skilled in the art.
[0031] The invention adjusts the coarse selenium slag to obtain the selenium slurry.
[0032] In the present invention, in terms of mass percentage, the coarse selenium slag preferably further inclu...
Embodiment 1
[0056] The coarse selenium slag comprises the following components in mass percentage: Se 75.04%, Te 7.08%, Pb 5.78%, Cu6.7%, water 3.9%, and the balance is other trace impurities and salts; the coarse selenium slag particle size is 100 ~200μm;
[0057] First, 1kg of coarse selenium slag and deionized water are mixed at a solid-to-liquid ratio of 1:1 to obtain selenium slurry;
[0058] Adjust the obtained selenium mud to a pH value of 1 with a mass fraction of 40% dilute sulfuric acid, add 209 mL of hydrogen peroxide with a mass concentration of 15% as an oxidant, and adjust the potential of the system to 500 mV. After fully stirring for 30 min, wash with water to The pH value of the system is 7, and after pressure filtration, it is placed in a vacuum drying oven and dehydrated under reduced pressure at 100°C and 500Pa to obtain primary selenium;
[0059] The obtained primary selenium was smelted at 400° C. for 60 minutes until the selenium powder was completely melted into a...
Embodiment 2
[0066] The coarse selenium slag includes the following components in mass percentage: Se 90.23%, Te 3.08%, Pb 1.20%, Cu1.7%, water 2.9%, and the balance is other trace impurities and salts; the coarse selenium slag particle size is 150 ~250μm;
[0067] First, 1kg of coarse selenium slag and deionized water are mixed at a solid-to-liquid ratio of 1:2 to obtain selenium slurry;
[0068] Adjust the obtained selenium slurry to a pH value of 2 with a mass fraction of 30% dilute sulfuric acid, add 293 mL of hydrogen peroxide with a mass concentration of 15% as an oxidant, and adjust the potential of the system to 550 mV. After fully stirring for 50 min, wash with water to The pH value of the system is 7, and after pressure filtration, it is placed in a vacuum drying oven and dehydrated under reduced pressure at 100°C and 500Pa to obtain primary selenium;
[0069] The obtained primary selenium was smelted at 350° C. for 90 minutes until the selenium powder was completely melted into...
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