Method for preparing high-purity selenium from crude selenium product

A technology of high-purity selenium and crude selenium, applied in the direction of element selenium/tellurium, etc., can solve the problems of large reagent consumption, high production cost, and long process flow, and achieve simple and practical process, good selenium purification effect, and good environmental protection Effect

A technology of high-purity selenium and crude selenium, applied in the direction of element selenium/tellurium, etc., can solve the problems of large reagent consumption, high production cost, and long process flow, and achieve simple and practical process, good selenium purification effect, and good environmental protection Effect

CN110316705AActive Publication Date: 2019-10-11云南铜业科技发展股份有限公司
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  • Method for preparing high-purity selenium from crude selenium product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A. Take 1Kg of crude selenium material from a smelter, its main components (mass percentage) are: Se 97.36%, Te1.28%, Cu 0.028%, Pb 0.014%. The material is crushed to a particle size below 3mm, dried and placed in a quartz tube furnace. Start the furnace to raise the temperature to 550°C, and at the same time turn on industrial high-purity dry oxygen, and the oxygen flow rate is controlled at 1L / min. When the furnace temperature reaches 550°C, keep it warm for 10 minutes, turn off the oxygen, and turn off the furnace to cool naturally;

[0026] B. arrange and collect the condensed selenium dioxide crystals, remove the slag in the furnace, and continue to heat up to 500°C in the quartz tube furnace for sublimation. When the furnace temperature reaches 500°C, keep the temperature for 15 minutes. Then lower the furnace temperature control to 200°C for natural condensation. When the furnace temperature reaches 200°C, keep the temperature for 10 minutes and then open the fu...

Embodiment 2

[0031] A. Get 2Kg of crude selenium material from a smelter, its main components (mass percentage) are: Se 98.32%, Te1.26%, Cu 0.023%, Pb 0.012%. The material is crushed to a particle size below 3mm, dried and placed in a quartz tube furnace. Start the furnace to raise the temperature to 575°C, and at the same time turn on industrial high-purity dry oxygen, and the oxygen flow rate is controlled at 1.2L / min. When the furnace temperature reaches 575°C, keep it warm for 10 minutes, turn off the oxygen, and turn off the furnace to cool naturally;

[0032] B. arrange and collect the condensed selenium dioxide crystals, remove the slag in the furnace, and continue to heat up to 550°C in the quartz tube furnace for sublimation. When the furnace temperature reaches 550°C, keep the temperature for 15 minutes. Then lower the furnace temperature control to 205°C for natural condensation. When the furnace temperature reaches 205°C, keep the temperature for 10 minutes and then open the f...

Embodiment 3

[0037] A. Get 3Kg of crude selenium material from a smelter, its main components (mass percentage) are: Se 98.97%, Te1.24%, Cu 0.022%, Pb 0.012%. The material is crushed to a particle size below 3mm, dried and placed in a quartz tube furnace. Start the furnace to raise the temperature to 600°C, and at the same time turn on industrial high-purity dry oxygen, and the oxygen flow rate is controlled at 1.4L / min. When the furnace temperature reaches 600°C, keep it warm for 10 minutes, turn off the oxygen, and turn off the furnace to cool naturally;

[0038] B. arrange and collect the condensed selenium dioxide crystals, remove the slag in the furnace, and continue to heat up to 600°C in the quartz tube furnace for sublimation. When the furnace temperature reaches 600°C, keep the temperature for 15 minutes. Then lower the furnace temperature control to 210°C for natural condensation. When the furnace temperature reaches 210°C, keep warm for 10 minutes and then open the furnace exha...

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Abstract

The invention relates to a method suitable for further purifying a crude selenium product with the selenium mass percent of 97-99% to prepare high-purity selenium with the grade of 99.999% or above, and belongs to the technical field of nonferrous metallurgy engineering. The preparation method includes the steps that a crude selenium material is crushed until the particle size is 3 mm or below, the crude selenium material is placed in a quartz tube furnace for oxidative distillation, and the furnace temperature is controlled to be 550-600 DEG C; sublimation and recondensation are performed inthe furnace after condensation, and the furnace temperature is controlled to be 500-600 DEG C; then, the material is conveyed into a glass-lined reactor, and deionized water is added for a water-soluble reaction; the solution is filtered through a bag filter and then placed in the glass-lined reactor, hydrazine hydrate with the concentration of 10-15% is dropwise added, and a generated paste-likeprecipitate is collected to obtain the high-purity selenium product. The whole technical method for preparing the high-purity selenium has the advantages of short flow, airtightness and no pollution,and thus the high-purity selenium product meeting the Se99.999 and Se99.9999 brand standard can be prepared with high efficiency, environmental protection and energy conservation.

Description

technical field [0001] The invention relates to a preparation method suitable for further purifying crude selenium products (containing Se in a mass percentage of 97-99%) to high-purity selenium containing more than 99.999% of Se, belonging to the technical field of nonferrous metal extraction metallurgical engineering. Background technique [0002] High-purity selenium materials generally refer to metal materials with high chemical purity and low impurity content containing more than Se99.999%, which are mainly used in the manufacture of compound semiconductors, thermoelectric conversion, photosensitive materials, thin-film materials for infrared detection, and solar cell materials. High-tech development product field. [0003] The methods for further purification of crude selenium mainly include vacuum distillation, ion exchange, thermal decomposition of selenides, gas-phase ammonia reduction of selenium dioxide or combined methods, etc. High, causing new environmental pr...

Claims

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Application Information

Patent Timeline
11 Oct 2019
Publication
CN110316705A
IPC
C01B19/02
CPC
C01B19/02
Inventors
赵群; 商仕杰